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  • Inorganic Chemistry  (1,324)
  • 1995-1999  (567)
  • 1980-1984  (757)
  • 1955-1959
  • 1925-1929
  • 1995  (567)
  • 1980  (757)
Collection
Keywords
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  • 1995-1999  (567)
  • 1980-1984  (757)
  • 1955-1959
  • 1925-1929
Year
  • 1
    Electronic Resource
    Electronic Resource
    2,2-Disubstituierte 1,3-Dithiane aus β-Dicarbonylverbindungen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 800-805 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2,2-Disubstituted 1,3-Dithianes from β-Dicarbonyl Compounds1,3-Dicarbonyl compounds 2 can be condensed with 1,3-propanedithiol (1) to yield 2,2-disubstituted 1,3-dithianes 3 which are remarkably stable in contrast to analogous open-chain thioacetals 6. Compounds with alkoxycarbonyl functions are easily hydrolysed to the corresponding carboxylic acids 11 which by further esterification with alkanols 12 yield estermodified 1,3-dithianes 3. All new compounds are characterized by 13C NMR spectroscopy.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130238
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  • 2
    Electronic Resource
    Electronic Resource
    Perchlor-2-methylen-2H-pyran (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 806-807 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Perchloro-2-methylene-2H-pyranThe synthesis of the title compound 4 is described. 4 is thermally and chemically very stable.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130239
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  • 3
    Electronic Resource
    Electronic Resource
    Anchimer beschleunigte Homolysen, V. Thermische und Fluoridionen-katalysierte Umlagerungen von Benzyl)-[9-(trimethylgermyl)-9-fluorenyl]-ether (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 808-810 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Anchimerically Enhanced Homolyses, V. Fluoride Ion Catalysed Rearrangements of Benzyl 9-(Trimethylgermyl)-9-fluorenyl EtherThe thermal rearrangement (homolysis) of the germanium compound 1d into 4d is considerably slower than that of the analogous Si compound 1c. Thus, a correlation is suggested between the velocity of the rearrangement and the strength of the new bond to oxygen. The rearrangement 1d→4d is also induced by fluoride ions at room temperature.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130240
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  • 4
    Electronic Resource
    Electronic Resource
    Masthead (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130301
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  • 5
    Electronic Resource
    Electronic Resource
    Thion- und Dithioester, XXII. α,β-Ungesättigte Thion- und Dithioester (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 919-933 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thiono and Dithio Esters, XXII. α,β-Unsaturated Thiono and Dithio Estersα,β-Unsaturated thiono and dithio esters such as O-ethyl thiocinnamate (3), methyl dithiocinnamate (7), O-ethyl thiocrotonate (17), and O,O-diethyl dithiofumarate (28) have been prepared by thiolysis between 20 and -75°C from the corresponding O- or S-alkylated tertiary amides or thioamides. They tend to dimerize in part by [4 + 2] cycloadditions. Methyl dithiocrotonate (24) could only be isolated as the endo-dimer 25.
    Notes: α,β-Ungesättigte Thion- und Dithioester wie Thiozimtsäure-O-ethylester (3), Dithiozimtsäure-methylester (7), Thiocrotonsäure-O-ethylester (17) und Dithiofumarsäure-O,O-diethylester (28) sind durch Thiolyse aus den entsprechenden O- oder S-alkylierten tertiären Amiden oder Thio-amiden bei Temperaturen von 20 bis -75°C zugänglich. Sie dimerisieren zum Teil in [4 + 2]-Cycloadditionen. Dithiocrotonsäure-methylester (24) ist nur als endo-Dimeres 25 erhältlich.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130312
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  • 6
    Electronic Resource
    Electronic Resource
    Zur Thermolyse von Verbindungen mit geometrisch fixierter Vinyloxiran-Einheit: Stereospezifische Synthese von 4,5-anellierten cis- und trans-2,3-Dihydrofuranen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 875-901 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermolysis of Compounds with a Geometrically Fixed Vinyloxirane Unit: Stereospecific Synthesis of 4,5-Fused cis-and trans-2,3-DihydrofuransThe conformationally fixed vinyloxiranes 7c - f, 8a - f, and 9b - d are transformed thermally into the bicyclic ethers 23 - 25. Starting with the spiro-derivatives c - f, which are monosubstituted at the vinyl group, the ring expansion takes place with high stereospecificity leading to 4,5-fused cis-(c/e) and trans-2,3-dihydrofurans (d/f), respectively. On heating 8b and 9b in the presence of dimethylfumarate besides the isomerisation to 24b/25b two cycloadducts are formed in each case to which the structures of 29/31 and 30/32 have been assigned. Oxapentadienyl dipoles (3) are proposed as intermediates in which the rotation of C/O-bonds is energetically more favorable than rotation of C/C-bonds. The activation parameters for the transformation 8b → 24b are determined and discussed together with the reported data of some analogous ring expansion reactions.
    Notes: Die konformativ fixierten Vinyloxirane 7c - f, 8a - f und 9b - d wandeln sich thermisch mit Ausbeuten zwischen 50 und 80% in die bicyclischen Ether 23 - 25 um. Ausgehend von den an der Vinylgruppe monosubstituierten Spiro-Derivaten c - f erfolgt die Ringerweiterungsreaktion mit hoher Stereospezifität zu 4,5-anellierten cis- (c/e) bzw. trans-2,3-Dihydrofuranen (d/f). Beim Erhitzen von 8b und 9b in Gegenwart von Fumarsäuredimethylester entstehen neben den Isomeren 24b bzw. 25b jeweils zwei Cycloaddukte im Verhältnis 10: 1, denen die Strukturen 29/31 und 30/32 zugeordnet werden. Als Zwischenstufen werden Oxapentadienyl-Dipole (3) angenommen, in welchen die Rotation um C/O-Bindungen energetisch günstiger ist als die um C/C-Bindungen. Die Aktivierungsparameter der Umwandlung 8b → 24b werden bestimmt und im Zusammenhang mit denen einiger analoger Ringerweiterungen diskutiert.
    Additional Material: 12 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130309
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  • 7
    Electronic Resource
    Electronic Resource
    Statistische Synthesen von Rotaxanen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 941-954 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Statistical Syntheses of RotaxanesThe acetalisation of the 28-membered cyclic diols 11a, b with the long-chain dibromo ketone 12 gives acetals 13a, b. These compounds react with triphenylmethyllithium to give 17a, b and 18a, b from which the rotaxanes 20a, b are obtained in 0.066 or 0.18 and 0.12% yield, respectively, after hydrolysis of the acetal bonds. The reacetalisation of rotaxane 20b affords, by an intraannular reaction, the prerotaxane 18b in pure form.
    Notes: Die Acetalisierung der 28-gliedrigen cyclischen Diole 11a, b mit dem langkettigen Dibromketon 12 ergibt die Acetale 13a, b. Nach Umsetzung mit Triphenylmethyllithium zu 17a, b und 18a, b werden nach Hydrolyse der Acetalbindungen die Rotaxane 20a, b in Ausbeuten von 0.066 und 0.18 bzw. 0.12% als farblose Öle isoliert. Durch Reacetalisierung von 20b wird in einer intraannularen Reaktion das Prärotaxan 18b in reiner Form erhalten.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130314
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  • 8
    Electronic Resource
    Electronic Resource
    Umlagerung von α-Isocyanato-N2-(arylsulfonyl)amidinen in 1-Arylsulfonyl-3-imidazolin-2-one (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 934-940 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rearrangement of α-Isocyanato-N2-(arylsulfonyl)amidines to 1-Arylsulfonyl-3-imidazolin-2-onesThe reaction of the azirines 1 with the isocyanates 2 leads to the α-isocyanato-N2-(arylsulfonyl)-amidines 6. Starting from 1b, also considerable amounts of 7b and 8b are formed as a result of a retro-ene reaction of 6b. The heterocumulenes 6 readily rearrange with a shift of the sulfonyl group to give the heterocycles 10. The mobility of the sulfonyl residue is also obvious from the reaction of 6a with hydrogen chloride to afford tosyl chloride and 8a as well as from the reaction with amines, which, however, does not only yield the tosylamides 15, but also the ureas 13 and their secondary products 14.
    Notes: Die Reaktion der Azirine 1 mit den Isocyanaten 2 führt zu den α-Isocyanato-N2-(arylsulfonyl)-amidinen 6. Ausgehend von 1b werden auch beträchtliche Mengen 7b und 8b als Folge einer Retro-En-Reaktion von 6b gebildet. Die Heterocumulene 6 lagern sich unter Wanderung der Sulfonyl-Gruppe leicht in die Heterocyclen 10 um. Die Beweglichkeit des Sulfonyl-Rests wird auch in der Reaktion von 6a mit Chlorwasserstoff zu Tosylchlorid und 8a sowie in der Umsetzung mit Aminen deutlich, die neben Tosylamiden 15 allerdings auch Harnstoffe 13 und deren Folgeprodukte 14 liefert.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130313
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  • 9
    Electronic Resource
    Electronic Resource
    Di-μ-(carboxylato)-bis[dicarbonyl(tri-tert-butylphosphan)-ruthenium(I)](Ru - Ru) (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 989-994 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Di-μ-(carboxylato)-bis[dicarbonyl(tri-tert-butylphosphane)ruthenium(I)](Ru - Ru)Ru3(CO)12 reacts with tri-tert-butylphosphane and formic acid, acetic acid, propionic acid, butyric acid, or stearic acid to form di-μ-(carboxylato)-bis[dicarbonyl(tri-tert-butylphosphane)-ruthenium(I)](Ru - Ru). The IR and NMR spectroscopic data are discussed.
    Notes: Ru3(CO)12 reagiert mit Tri-tert-butylphosphan und Ameisensäure. Essigsäure, Propionsäure, Buttersäure oder Stearinsäure unter Bildung von Di-μ-(carboxylato)-bis[dicarbonyl(tri-tert-butylphosphan)ruthenium(I)](Ru - Ru). Die IR- und NMR-spektroskopischen Daten der neuen Komplexe werden diskutiert.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130318
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  • 10
    Electronic Resource
    Electronic Resource
    Addition von Aldehyden an aktivierte Doppelbindungen, XXIII. Synthesen von 1,3,6-Triketonen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 979-988 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Addition of Aldehydes to Activated Double Bonds, XXIII. Syntheses of 1,3,6-TriketonesThiazolium salt-catalyzed addition of aldehydes to monoacetals of vinyl-1,3-diketones (1, 2; 23, 24) leads to 1,4-diketones (3 - 10; 25 - 31), which are hydrolyzed to 1,3,6-triketones (11 - 18; 32 - 38). A way to the mono-acetalized vinyl-1,3-diketones 1, 2; 23, 24 using the norbornenyl group with following pyrolysis is given.
    Notes: Thiazoliumsalz-katalysierte Additionen von Aldehyden an mono-acetalisierte Vinyl-1,3-diketone (1,2; 23, 24) führen zu 1,4-Diketonen (3 - 10; 25 - 31), die sich zu den 1,3,6-Triketonen (11 - 18; 32 - 38) hydrolysieren lassen. Ein Syntheseweg zu den mono-acetalisierten Vinyl-1,3-diketonen 1, 2; 23, 24 über die Norbornenyl-Gruppierung und nachfolgende Pyrolyse wird angegeben.
    Additional Material: 6 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130317
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  • 11
    Electronic Resource
    Electronic Resource
    Einführung der (Dimethylhydrazono)ethylgruppe in methylenaktive Verbindungen und Phenole (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 970-978 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Introduction of the (Dimethylhydrazono)ethyl Group into Methylene Active Compounds and PhenolsIn [2-(dimethylhydrazono)ethyl]trimethylammonium iodide the trimethylammonium group can be substituted by several nucleophiles. With this reagent (dimethylhydrazono)ethyl derivatives of CH-acidic compounds, phenols, and indole can be prepared.
    Notes: In [2-(Dimethylhydrazono)ethyl]trimethylammonium-iodid (19) läßt sich die Trimethylammoniumgruppe durch verschiedenartige Nucleophile verdrängen. CH-acide Verbindungen sowie Phenole und Indole kann man mit diesem Reagenz zu den entsprechenden Hydrazonoethyl-Derivaten umsetzen.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130316
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  • 12
    Electronic Resource
    Electronic Resource
    Synthese neuer Mono- und Disaccharidglycale zum Aufbau von Oligodesoxyoligosacchariden (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 955-969 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Novel Mono- and Disaccharide Glycals for the Synthesis of Oligodeoxy OligosaccharidesUnder various conditions opening of the 6-deoxy-allo-epoxide 1 with lithium iodide yields a mixture of the 3-iodo-gluco-(3) and, predominantly, the 2-iodo-altro-hydrine (2), the reaction of which with methyllithium is studied. By a simplified procedure rendering a separation of 2a and 3a unnecessary the preparation of crystalline D-digitoxal (4a) in approximately 50% yield based on 1 is described. The condensation of 1 and 4b in the presence of N-iodosuccinimide yields the α,1→4-linked altro-allo disaccharide derivative 8a, and only minor amounts of the isomeric β,1→4-linked allo-allo disaccharide 10. Following the opening of the epoxide ring in 8a with lithium iodide and subsequent separation of the iodo hydrines by reduction of the bis-altro derivative 11a a synthesis of the methyl glycoside of the terminal disaccharide (12a) in neodigoxin is achieved. Starting with a reduction of 8a to 13b the subsequent opening of the epoxide ring with lithium iodide and separation of the isomers gives an access to the ribo-altro derivative 16b. By its reaction with methyllithium the disaccharide glycal digitoxosyl-digitoxal 15a is synthesized. The linkage of 15b with 1 is effected by application of the N-iodosuccinimide procedure and yields the trisaccharide derivative 17. The structures and conformations of all derivatives are characterized by comprehensive 1H NMR spectroscopy.
    Notes: Die Öffnung des 6-Desoxy-allo-epoxid-Derivats 1 mit Lithiumiodid gibt unter verschiedenen Bedingungen ein Gemisch aus dem 3-Iod-gluco-(3) und überwiegend dem 2-Iod-altro-Hydrin (2), deren Umsetzungen mit Methyllithium untersucht werden. Ein vereinfachtes Verfahren ermöglicht ohne Trennung von 2a und 3a die Herstellung des kristallinen D-Digitoxals (4a) mit ca. 50% Ausbeute, bezogen auf 1. Die Kondensation von 1 mit 4b und N-Iodsuccinimid gibt glatt das α,1→4-verknüpfte altro-allo-Disaccharid-Derivat 8a und nur in geringen Mengen das isomere β,1→4-gebundene allo-allo-Disaccharid 10. Nach Öffnung des Epoxidringes in 8a mit Lithiumiodid und Trennung der Iodhydrine wird durch Reduktion des bis-altro-Derivats 11a das Methylglycosid des terminalen Disaccharids (12a) aus Neodigoxin gewonnen. Durch vorgelagerte Reduktion von 8a zu 13b läßt sich nach Öffnung des Epoxidringes mit Lithiumiodid und Trennung der Isomeren aus dem ribo-altro-Derivat 16b mit Methyllithium das Disaccharidglycal Digitoxosyl-digitoxal 15a darstellen. Die Verknüpfung von 15b mit 1 nach dem N-Iodsuccinimid-Verfahren liefert das Trisaccharid-Derivat 17. Alle Derivate wurden hinsichtlich der Struktur und Konformation durch 1H-NMR-Spektren charakterisiert.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130315
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  • 13
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    Electronic Resource
    Übergangsmetall-Carbin-Komplexe, LII. (Tricarbonylchrom)-η;6-phenyl als Substituent in Carben- und Carbinkomplexen der VI. Nebengruppe (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 1010-1019 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Carbyne Complexes, LII. (Tricarbonylchromium)-η6-phenyl as Substituent in Carbene- and Carbyne Complexes of the VI. SubgroupThe reaction of tricarbonyl(η6-phenyllithium)chromium with the metalhexacarbonyls of the VI. subgroup and subsequent alkylation by triethyloxonium tetrafluoroborate yields pentacarbonyl-{ethoxy[(tricarbonylchromium)-η6-phenyl]carbene} complexes of chromium, molybdenum, and tungsten (1 - 3). 1 and 3 react with boron trihalides BX3 (X = Cl, Br) by cleavage of the ethoxy group to form trans-tetracarbonylhalogeno[(tricarbonylchromium)-η6-phenylcarbyne]metal complexes 4 - 7. Properties, spectroscopic results, and the X-ray structure analysis of 6 are discussed.
    Notes: Die Umsetzung von Tricarbonyl(η6-phenyllithium)chrom mit den Metallhexacarbonylen der VI. Nebengruppe und anschließende Alkylierung mittels Triethyloxonium-tetrafluoroborat führt zu Pentacarbonyl{ethoxy[(tricarbonylchrom)-η6-phenyl]carben}-Verbindungen des Chroms, Molybdäns und Wolframs (1 - 3). 1 und 3 reagieren mit den Bortrihalogeniden BX3 (X = Cl, Br) unter Abspaltung der Ethoxygruppe zu den trans-Tetracarbonylhalogeno[(tricarbonylchrom)-η6-phenylcarbin]metall-Komplexen 4 - 7. Eigenschaften und spektroskopische Ergebnisse sowie die Röntgenstrukturanalyse von 6 werden diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130320
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  • 14
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    Electronic Resource
    Beiträge zur Chlorierung - Dehydrochlorierung von Perhydro-1,4-thiazepin-5-onen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 995-1009 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chlorination - Dehydrochlorination of Perhydro-1,4-thiazepin-5-onesThe synthesis of unsaturated derivatives of perhydro-1,4-thiazepin-5-ones 3 is investigated. Depending on the substitution the thiazepin-5-ones 3 thereby react with sulfuryl chloride to yield 7- and 2-chloro derivatives 6 and 7; the latter eliminate hydrogen chloride only in the presence of a base (PVP, 8) to give the Δ2-thiazepines 9a,b,d,e,g, whereas the 7-chloro derivatives in situ afford the Δ6-thiazepines 10a - f, the 1,4-thiazepinium chloride 11c being isolated as intermediate. tert-Butyl hypochlorite forms according to the substituent size and solvent polarity 2- and 7-halogenation products, as well as 1,4-thiazepin-5-one-S-oxides 22. Further halogenation of the Δ6-1,4-thiazepines 10a - c results in the formation of unsaturated halogen derivatives 24, 25, and 26.
    Notes: Es wird versucht, ungesättigte Derivate von Perhydro-1,4-thiazepin-5-onen 3 herzustellen. Die Thiazepin-5-one 3 reagieren dabei je nach Substitution mit Sulfurylchlorid zu 7- und 2-Chlorderivaten 6 und 7; letztere eliminieren Chlorwasserstoff erst in Basen-Gegenwart (PVP, 8) zu den Δ2-Thiazepinen 9a,b,d,e,g, die 7-Chlorderivate dagegen in situ zu den Δ6-Thiazepinen 10a - f, wobei das 1,4-Thiazepinium-chlorid 11c in Substanz erhalten wird. tert-Butylhypochlorit ergibt je nach Substituentengröße und Solvenspolarität neben 2- und 7-Halogenierung auch durch Umlagerung 1,4-Thiazepin-5-on-S-oxide 22. Erneute Halogenierung der Δ6-1,4-Thiazepine 10a - c ergibt die ungesättigten Halogenderivate 24, 25 und 26.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130319
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  • 15
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    Electronic Resource
    Zur Kenntnis organischer Lewis-Säuren, 34. Die thermische [4π + 2π]-Cycloaddition von Enolethern an 1,1-dicarbonylsubstituierte Ethene (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 1020-1032 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organic Lewis Acids, 341. Thermal [4π + 2π]-Cycloaddition of Enol Ethers to 1,1-Dicarbonyl Substituted EthenesEnol ethers such as ethyl vinyl ether and 1,1-dimethoxyethene (3f) react thermally, in some instances below 0°C, with cyclic 2-alkylidene-1,3-dicarbonyl compounds such as 1 and 2 to give [4π + 2π]-cycloadducts 4 and 5, respectively (cyclic enol acetals and enol orthoesters), and with 1,1-dicyanoethenes 6 to give [2π + 2π]-cycloadducts 7. On passing from toluene to acetonitrile as the solvent, rates of formation of 4bf from 1b and 3f increase about tenfold and those of 7b from 6b and 3f about sixfold. A discussion of these rates, including rates of related reactions, the relative Lewis acid strengths of 1b and 6b, and the behaviour of 1b/3f towards methanol leads to the conclusion that the degree of concert of the formation of 4bf is below 6.5 kJ · mol-1. - The configurations and conformations of adducts 4 and 5 are discussed.
    Notes: Enolether wie Ethylvinylether und 1,1-Dimethoxyethen (3f) bilden mit exocyclisch 1,1-dicarbonylsubstituierten Ethenen wie 1 und 2 z.T. schon unterhalb von 0°C thermisch die [4π + 2π]-Addukte 4 bzw. 5 (cyclische Enolacetale und Enolorthoester) und mit den 1,1-Dicyanethenen 6 die [2π + 2π]-Addukte 7. Die Bildungsgeschwindigkeit von 4bf aus 1b und 3f steigt auf etwa das Zehnfache und die von 7b aus 6b und 3f auf etwa das Sechsfache beim Übergang von Toluol auf Acetonitril als Lösungsmittel. Eine Diskussion dieser Bildungsgeschwindigkeiten unter Einbeziehung verwandter Reaktionsgeschwindigkeiten sowie der relativen Lewis-Säurestärken von 1b und 6b und des Verhaltens des Systems 1b/3f gegenüber Methanol führt zum Schluß, daß der energetische Konzertiertheitsgrad der Bildung von 4bf unter 6.5 kJ · mol-1 liegt. Die Konfigurationen und Konformationen der Addukte 4 und 5 werden diskutiert.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951280101
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    Tripodal Triamidostannates as Building Blocks in the Generation of Sn - M-Bonded Heterobimetallics (M = Fe, Ru) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 29-34 
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    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Triamidostannates ; Metal-metal bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By in situ lithiation of the trifunctional amines H3CC(CH2NHSiMe3)3, PhC(CH2NHSiMe3)3, and HC{SiMe2NH(p-Tolyl)}3 and subsequent reaction with SnCl2 the corresponding triamidostannates were obtained. These were coupled with CpM(CO)2Cl (M = Fe, Ru) to yield the M - Sn-bonded heterobimetallics 9-14 of which H3CC(CH2NSiMe3)3SnFe(CO)2Cp (9) was characterized by a single-crystal X-ray structure analysis. Of the in situ-generated amidostannates only [HC{SiMe2N(p-Tolyl)}3Sn][Li(THF)3] (8) could be isolated as a uniform product and characterized analytically and spectroscopically.
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    The Structures of [X2Y—N—YX2]+ Cations (X = F, Cl; Y = S, Se). A Comparison of X-ray and ab Initio Studies[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 35-40 
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    ISSN: 0009-2940
    Keywords: Selenium-nitrogen compounds ; Sulfur-nitrogen compounds ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structures of cationic species of the series [X2Y—N—YX2]+ (X = F, Cl; Y = S, Se) have been computed ab initio using all electron treatments for first-row elements and sulfur and quasi-relativistic pseudopotentials for Se and Cl. Splitvalence basis sets with polarization and diffuse functions were employed. The MP2 results for the (non-isostructural!) cations [Cl2Se—N—SeCl2]+ (1: Cs) and [F2S—N—SF2]+ (2: C2v) are in excellent agreement with the experimental (X-ray) observations. Both structures represent local minima. A deeper minimum for either of the cations is represented by another C2v isomer which for crystal lattice energy reasons is stable in the isolated state only. The geometries of the hitherto unknown species [Cl2S—N—SCl2]+ (3) and [F2Se—N—SeF2]+ (4) have been assessed by ab initio HF calculations. In analogy to 2, cations 3 and 4 are predicted to prefer C2v symmetry. Therefore, 1 exhibits unusual structural features. According to strictly localized natural bond orbital analysis (NBO), the central nitrogen atoms in 1 and 2 possess two lone pairs of electrons (LP: one sp hybrid and one p orbital). The relatively short Se—N and S—N bond distances in 1 (1.741-1.760 Å) and 2 (1.551 Å) can best be attributed to LP(N)→s̰*(Y—X) negative hyperconjugation (1: Y = Se, X = Cl; 2: Y = S, X = F).
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    Die fördernde Rolle von Phosphinoester-Liganden bei der Synthese neutraler Carben-, Vinyliden- und Allenyliden-Ruthenium(II)-KomplexeHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 49-62 
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    ISSN: 0009-2940
    Keywords: Ruthenium(II) complexes, octahedral ; Phosphino esters as mono- and bidentate ligands ; Fluxional behaviour ; Carbene complexes ; Vinylidene complexes ; Allenylidene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vinylidene Transition-Metal Complexes, XXXV[1].  -  The Supporting Role of Phosphino Ester Ligands for the Synthesis of Neutral Carbene, Vinylidene and Allenylidene Ruthenium(II) ComplexesThe reaction of [RuCl2(PPh3)3] (1) with the phosphino esters iPr2P(CH2)nCO2R (2-4) leads to complete (n = 1; R = CH3, C2H5) or partial (n = 2; R =CH3) displacement of the PPh3 ligands and formation of the octahedral ruthenium(II) complexes [RuCl2{k2(P,O)-iPr2PCH2CO2R}2] (5, 6) and [RuCl2(PPh3){k(P)-iPr2PCH2CH2CO2Me}{k2(P,O)-iPr2PCH2CH2CO2Me}] (7). Treatment of 5 with LiBr and LiI affords the dibromo- and diiodoruthenium derivatives 8 and 9. While compound 5 reacts with CO and SO2 by cleavage of one Ru - O bond to yield the 1:1 adducts [RuCl2(L){k(P)-iPr2PCH2CO2Me}{k2(P,O)-iPr2PCH2CO2Me}] (10, 11), the reaction of the dibromo derivative 8 with CO in solution gives the dicarbonyl complex [RuBr2(CO)2{k(P)-iPr2PCH2CO2Me}2](13). If CO is passed over 8 in the solid state, the corresponding monocarbonyl compound 14 is formed. The hydridoruthenium(II) complex 16, which is obtained from equimolar amounts of [RuHCl(CO)(PiPr3)2] (15) and 2, reacts with HC≡CMe by insertion to give the vinyl derivative [RuCl{E - CH=CHMe}(CO)(PiPr3){k2(P,O)-iPr2CH2CO2Me}] (17). Treatment of 5 with HC̊' (R' = H, Me, tBu, Ph) and of 6, 8, 9 with HC≡CPh affords upon photochemical activation the octahedral vinylidene complexes [RuX2-(=C=CHR){k(P)-iPr2PCH2CO2R}{k2(P,O)-iPr2PCH2CO2R}] (18-21 and 23-25) in good to excellent yield. At room temperature, these compounds (with the exception of 25) are highly fluxional in solution. From 31P-NMR measurements, the free energies of activation ΔG
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    Reaktionen von R2Al—AlR2 (R = CH(SiMe3)2) mit Trimethylsilylazid  -  Insertion in die Al—Al-Bindung und Abbau zum trimeren Dialkylaluminiumazid (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 81-85 
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    ISSN: 0009-2940
    Keywords: Aluminium-aluminium bond ; Insertion of trimethylsilyl azide ; Trimeric dialkylaluminium azide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of R2Al—AlR2 (R = CH(SiMe3)2) with Trimethylsilyl Azide  -  Insertion into the Al—Al Bond and Formation of a Trimeric Dialkylaluminium AzideTetrakis[bis(trimethylsilyl)methyl]dialuminium(4) (1) reacts with trimethylsilyl azide under insertion of one nitrogen atom into the Al—Al bond. As shown by NMR spectra and crystal structure the product contains three and four coordinated Al atoms due to the coordination of the α-nitrogen atom of the azide group to one of the Al atoms. An electronically delocalized N3-system is formed with a N—N bond length of 132.0 pm and a bond order of 1.5 for both N—N bonds. With an excess of trimethylsilyl azide further reaction is observed only under mild irradiation conditions with an exchange of the azide group between Si and Al and formation of Me6Si2 and the dialkylaluminium azide 3, which is better synthesized by the reaction of Me3Si—N3 with Cl—Al[CH(SiMe3)2]2. The sterically highly shielded aluminium azide 3 is a trimer in the solid state showing a non-planar 12-membered Al3N9 heterocycle with short N—N bonds (114 pm).
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    URL: http://dx.doi.org/10.1002/cber.19951280112
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    Transition-Metal Complexes with the Novel Scorpionate Ligand Dihydrobis-(tetrazolyl)borate: Synthesis and Characterization of Infinite Two-Dimensional Metal-Ligand Frameworks and One-Dimensional Water SubstructuresDedicated to Professor Dr. Herbert Schumann on the occassion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 323-328 
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    ISSN: 0009-2940
    Keywords: Poly(azolyl)borates, metal complexes of ; Bis(tetrazolyl)borate, metal complexes of ; Metal-nitrogen coordination ; Coordination polymers ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dihydrobis(tetrazolyl)borate metal compounds of the composition [M(L)2{μ-H2B(CHN4)2}2]n for M = Mn, Fe, Co, Zn, Cd with L = H2O and for M = Cu with L = NH3 are obtained from metal salts and K[H2B(CHN4)2]. Single-crystal X-ray studies reveal the formation of two-dimensional rhombic grid sheets through the bridging action of the bis(tetrazolyl)borate ligands. Each metal atom is octahedrally coordinated with two trans L ligands and four H2B(CHN4)-2 nitrogen donors. Two additional, hydrogen-bonded water molecules occupy the rhombic openings in the compounds with M = Mn, Fe, Co, Zn, and Cd. The water of crystallization is held in place through hydrogen bonding from the water ligands and to the nitrogen atoms to give a substructure of parallel kinked water chains. Temperature-variable magnetic measurements show a Curie-Weiss behavior for the paramagnetic complexes with M = Mn, Fe, Co, and Cu.
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    New Organophosphorus Ligands: Cyclopropanation and Other Reactions of Cumulenes Bearing Diphenylphosphanyl Substituents (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 365-371 
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    ISSN: 0009-2940
    Keywords: Cumulenes ; Butadienes ; Vinylcyclopropane ; Vinylidenecyclopropane ; Bicyclopropyl, phosphanyl-substituted ; Cyclopropanation ; Phosphane ligands ; Phosphane chalcogenides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Hydrophosphorylation of 1,4-bis(diphenylphosphanyl)butadiyne with diphenylphosphane leads to the butadiene (Ph2P)2C=CH—CH=C(PPh2)2 (1). Treatment of 1 with dimethylsulfonium methylide gives the vinylcyclopropane (Ph2P)2C=CH—CH(CH2)C(PPh2)2 (2). Compound 2 reacts with aqueous hydrogen peroxide, elemental sulfur, or selenium to afford the tetrachalcogenides (Ph2XP)2C=CH—CH(CH2)C(PXPh2)2 with X = O (3), X = S (4), X = Se (5), respectively. While the tetraphosphane 1 and the vinyl-cyclopropane compound 2 cannot be converted into a bis-(cyclopropyl) compound with an excess of Me2S=CH2, the tetrasulfide 4 readily affords a mixture of (1R,1′R)-/(1S,1′S)-and meso-2,2,2′,2′-tetrakis(diphenylthiophosphinyl)-1,1′-bicyclopropyl (6, 7) in good yield. Treatment of 1,1,4,4-tetrakis-(diphenylphosphanyl)butatriene with dimethylsulfonium methylide leads to the vinylidenecyclopropane (Ph2P)2C=C=C(CH2)C(PPh2)2 (8). Compound 8 is converted into its tetrasulfide (Ph2SP)2C=C=C(CH2)C(PSPh2)2 (9) by treatment with elemental sulfur. The crystal structures of 1, 2, 4, 7, and 8 have been determined by single-crystal X-ray diffraction.
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    URL: http://dx.doi.org/10.1002/cber.19951280408
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    Mono- und Diferriophosphane und -thioxophosphoraneHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 413-416 
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    ISSN: 0009-2940
    Keywords: Ferriophosphanes ; Ferriophosphoranes ; Thioxophosphane ligand ; Decarbonylation reaction ; Sulfurization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mono- and Diferriophosphanes and -thioxophosphoranesHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet.The substitution of organic substituents in phosphanes or thioxophosphoranes by the 17-electron fragments CpFe-(CO)2 (—Fp) leads to isolobal ferriophosphanes or -thioxophosphoranes. The mono- and diferriophosphanes FpnPPh3-n [n = 1 (3), 2 (4)] are obtained by deprotonation of the mono- and diferriophosphonium salts [FpnPPh3-nH]X [n = 1 (1), 2 (2)] with DBU. They are oxidized by sulfur giving the mono- and diferriothioxophosphoranes FpnPPh3-n(S) [n = 1 (5), 2 (6)]. Sulfide 5 arises also from the reaction of CpFe(CO)2Cl and Ph2PH(S)/DBU. The one-sided decarbonylation reaction of 6 leads to FpFp′PPh(S) (7, Fp′ = CpFeCO). The Fp substituents (17 electrons) in 3-7 coordinate as one-electron donors to the PhnP- or PhnP(S) units (n = 1, 2). The bridging functions in 4 and 6 are hitherto unknown. The molecular structures of the complexes 5-7 were determined by X-ray structure analyses.
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    About some Electrophilic Substitution Reactions with [(CF3S)3C+][AsF-6] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 435-436 
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    ISSN: 0009-2940
    Keywords: Trifluoromethylthio group ; Carbenium ions ; Diphenylmethane ; Dyes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(trifluoromethylthio)carbenium hexafluoroarsenate (1) reacts with N,N-dimethylaniline and anisole to form the corresponding diphenylmethanes 2, 3 with the SCF3 group at the methine carbon atom. During the reaction of 1 with benzene, compounds such as C6H5C(SCF3)3 and C6H5SCF3 are formed along with benzophenone, a product of hydrolysis of the diphenylmethane compound.
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    Synthesis and Structure of the First Dimetalated Diphosphane Disulfide [(η5-C5Me5)(CO)2FeP(H)(S)]2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 441-442 
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    ISSN: 0009-2940
    Keywords: Diphosphane disulfides ; Metallophosphoranes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first transition metal derivative meso-[(η5-C5Me5)(CO)2FeP(H)(S)]2 (2) of the unknown diphosphane disulfide [PH2(S)]2 results from treatment of (η5-C5Me5)(CO)2FePH2 (1) with 1.5 equivalents of elemental sulfur. Compound 2 was characterized by means of spectroscopy (IR, 31P, 31P{1H}, 13C{1H}, 1H NMR) as well as X-ray diffraction analysis.
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    Preparation and Molecular Structures of Tetrahydrofuran, Diethylene Diglycol Dimethyl Ether and 18-Crown-6 Complexes of Strontium and Barium TetrahydridoborateDedicated to Prof. Dr. Nils Wiberg on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 455-460 
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    ISSN: 0009-2940
    Keywords: Strontium bis(tetrahydridoborate)-2 tetrahydrofuran, chain polymer of ; Strontium bis(tetrahydridoborate)-bis(diglyme) ; Barium bis(tetrahydridoborate)-bis(diglyme) ; Strontium bis(tetrahydridoborate)-1,4,7,13,16-hexaoxacyclooctadecane ; Metal-hydrogen-boron bridges ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The strontium and barium tetrahydridoborate complexes M(BH4)2 · 2 diglyme and M(BH4)2 · 18-crown-6 (M = Sr, Ba) have been prepared from the solvates M(BH4)2 · 2 THF by ligand displacement. 11B-NMR and IR data reveal strongly polar bonding of the BH4 groups to the metal centers, and X-ray structural analyses of the diglyme and crown ether compounds show molecular units in which the BH4 group is in contact via three H atoms with the metal center. In contrast, M(BH4)2 · 2 THF compounds are chain polymers in the solid state, and each metal center is surrounded by 2 THF molecules in trans position and four BH4- groups each of which forms bridges with two metal centers. Estimations of the effective radius for the BH4 group indicate a high polarity for the M-BH4 interaction.
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    Photochemische Reaktionen von Übergangsmetall-Organyl-Komplexen mit Olefinen, 1312. Mitteilung: Lit.Photochemisch induzierte [5+2],homo[5+21-Cycloaddition von 3-Hexin an Tricarbonyl(η5-2,4-cycloheptadien-l-yl)mangan (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 515-518 
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    ISSN: 0009-2940
    Keywords: Manganese ; Cycloheptadienyl ; Alkyne ; [5+2],homo[5+2] Cycloadditions ; Tricyclo[5.3.1.04,10]undeca-2,5-dien-11-yl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Photochemical Reactions of Transition Metal Organyl Complexes with Olefins, 1312. Mitteilung: Lit. . - Photochemically Induced [5+2], homo[5+2] Cycloaddition of 3-Hexyne to Tricarbonyl(η 5-2,4-cycloheptadien-1-yl)manganeseTricarbonyl(η5-2,4-cycloheptadien-1-yl)manganese (1) reacts upon UV irradiation in hexane at 243 K with two equivalents of 3-hexyne (2) in successive [5+2],homo[5+2] cycloadditions to give tricarbonyl(η2:2:1-1,2,3,11-tetraethyltricyclo-[5.3.1.04,10]undeca-2,5-dien-11-yl)manganese (3). Its crystal and molecular structure was determined by an X-ray diffraction analysis, in solution it was studied also by IR and NMR spectroscopy.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951280601
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    1,4,2-Diazaphospholothiazoles and -pyridines by a Hantzsch-Type Condensation Using Chloromethyldichlorophosphane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 581-587 
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    ISSN: 0009-2940
    Keywords: Anellated azaphospholes ; Hantzsch-type [3 + 2] cyclocondensation ; Chloromethyldichlorophosphane ; Regioselectivity ; 31P-, 1H-, 13C-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The [3 + 2] cyclocondensation of 2-amino-1,3-thiazoline, 2-aminopyridines, 2- and 4-aminopyrimidines, 2-aminopyrazine, and 2-aminoquinoline with chloromethyldichlorophosphane in the presence of triethylamine yields regiospecifically 5,6-dihydrothiazolo[2,3-e][1,4,2]diazaphosphole (3), 1,4,2-diazaphospholo[4,5-α]pyridines (12), 1,4,2-diazaphospholo[4,5-α]pyrimidines (15), 1,4,2-diazaphospholo[4,5-e]pyrimidine (17), 1,4,2-diazaphospholo[4,5-α]pyrazine (19), and [1,4,2]diazaphospholo[4,5-α]quinoline (22), respectively. Using 2-amino-1,3-thiazole (4) and 2-aminobenzothiazoles 8, we obtained mixtures of the 1,5- and 4,5-anellated 1,4,2-diazaphospholes 5/6, 9a/10a and 9b/10b, while in the case of the methyl derivative 8c only the [1,4,2]diazaphospholo[5,4-b][1,3]benzothiazole 10c was formed. In the reaction of 2-aminothiazole and 2-aminopyrazine with Chloromethyldichlorophosphane the bis(diazaphospholo)-substituted chloromethylphosphanes 7 and 20 could be detected. The new anellated 1,4,2-diazaphospholes are colorless to pale yellow crystalline moisture-sensitive solids.
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    Reactions at Silicon-Silicon Bonds, V. Selective Trichlorosilylation of Alkyl(diorganylamino)chlorophosphanes with Hexachlorodisilane or with Trichlorosilane/Triethylamine. - Two Routes to New Functional Trichlorosilylphosphanes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 615-619 
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    ISSN: 0009-2940
    Keywords: Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of alkyl(diorganylamino)chlorophosphanes R(R2′N)PCl 1 (1a: R = tBu, R′ = Et, 1b: R = iPr, R′ = iPr; 1c: R = iPr, R′ = Ph) with hexachlorodisilane, afforded alkyl(diorganylamino)trichlorosilylphosphanes R(R2′N)PSiCl3 2 (2a: R = tBu, R′ = Et; 2b: R = iPr, R′ = iPr; 2c: R = iPr, R′ = Ph) and silicon tetrachloride. An intermediate formed in the reaction of 1b with hexachlorodisilane, the adduct iPr(iPr2N)(Cl)P-Si(Cl)3-SiCl3 (3b = 1b · Si2Cl6), was detected by 31P- and 29Si-NMR spectra that indicate pentacoordinated silicon bound to tetracoordinated phosphorus and tetracoordinated silicon. Trichlorosilylphosphanes 2 are also available from 1 under very mild conditions by reductive trichlorosilylation with trichlorosilane in the presence of triethylamine. Compounds 2 were identified analytically, by mass spectroscopy, multinuclear NMR, and an X-ray structure determination of 2c.
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    Reactions of Complex Ligands, LXIVPart LXIII: Ref.. Synthesis of 5,5′-Diphenyl-2,2′-bifuran, a Biaryl Compound with Remarkable Fluorescence Properties (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 641-643 
    Details
    ISSN: 0009-2940
    Keywords: Carbene ligands ; Tungsten complexes ; 2,2′-Bifuran ; Copper coupling reaction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 2-oxacyclic α,β-unsaturated carbene complex 1 reacts with an excess of dimethylamine to give the diphenylbifuran 2. The structure of 2 was established by independent synthesis from 2-phenylfuran (4) via regioselective lithiation and transmetalation to zinc and tin organometallics 6a-c and final oxidative copper coupling reactions.
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    URL: http://dx.doi.org/10.1002/cber.19951280618
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    Synthesis of 2- and 3-Stannolenes via Addition of Trimethyltin Alkoxides to 3-Diethylboryl-4-ethyl-1,1-dimethylstannole (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 679-687 
    Details
    ISSN: 0009-2940
    Keywords: Stannole, diethylboryl-substituted ; Trimethyltin alkoxides ; 2-, 3-Stannolenes, organometallic-substituted ; NMR, coupling constants, 2J(Sn,Sn), sign determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trimethyltin alkoxides (2) react stereoselectively with 3-diethylboryl-4-ethyl-1,1-dimethylstannole (1) via addition of the Me3Sn group to C(2) to the C(2) = C(3) bond and a 1,2 shift of an ethyl group from boron to C(3) to give the 2-stannolenes 3. The molecular structure of 3f' [R = (S)-2-Bu] was determined by single-crystal X-ray analysis, confirming the cis positions of the Et(RO)B and the Me3Sn group. These 2-stannolenes 3 undergo, upon heating to ca. 80°C, facile rearrangement by irreversible allylic migration of the Et(RO)B group to the 3-stannolenes 4 in which the cis positions of the boryl and the stannyl group are retained. All 2-stannolenes (in contrast to the 3-stannolenes) are readily deprotoborylated to give the 3-stannolene 5. The structures of 3, 4, and 5 follow conclusively from 1H-, 11B-, 13C-, and 119Sn-NMR spectra. The negative sign of the geminal coupling constants 2J(SnSn) was determined in the case of 3, 4, and 5 by 2D 119Sn/1H heteronuclear shift correlations.
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    Synthesis of Structures of (Acyloxy)boranesDedicated to Prof. Dr. A. Schmidpeter on the occasion of his 65th birthday.Synthesis of Structures of (Acyloxy)boranes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 751-762 
    Details
    ISSN: 0009-2940
    Keywords: Trifluoroacyloxy-9-borabicyclo[3.3.1]nonane ; Pivaloyloxy-9-borabicyclo[3.3.1]nonane dimer ; Bis(9-borabicyclo[3.3.1]nonyl]oxalate ; Tetrakis(9-borabicyclo[3.3.1]nonyl)-dihydroxyoxalate ; Bis(9-borabicyclo[3.3.1]nonyl)-2,2-dimethylmalonate tetramer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 9-Borabicyclo[3.3.1]nonane (9-BBNH) reacts with monocarboxylic acids to afford 9-(acyloxy)-9-borabicyclo[3.3.1]nonanes which are dimers in the solid state as shown by X-ray crystal structures of the benzoate and pivalate. More complex reactions were observed by allowing 9-BBNH to react with dicarboxylic acids in THF or monoglyme. Thus, (9-BBN)2 oxalate 3 contains a fully delocalized oxalate unit with equal C-O and B-O bond lengths. Traces of water convert it into the tetrakis(9-BBN) oxalate 5. A rather unusual structure is veryfied by 9-BBN 2,2-dimethylmalonate 7 which according to its molecular structure is a tetramer featuring a 32-membered ring system. In contrast, reactions of oxalic acid with thexylborane leads to reduction of the acid and formation of a bicyclic dioxaborolo-dioxaborolane 10. Several intermediates were detected by 11B-NMR spectroscopy as well as in reactions of BH3 · THF or BH3 · SMe2 with oxalic acid.  -  It follows from the present study that (acyloxy)boranes derived from dicarboxylic acids are strong Lewis acids with an unexpected variety of structural features.
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    A T-Shaped Selenenyl Halide: Synthesis and Characterisation of a Proposed Reaction Intermediate (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 741-742 
    Details
    ISSN: 0009-2940
    Keywords: Selenenyl halides ; Nucleophilic substitution ; Complex intermediate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The T-shaped selenenyl halide (1), which may be regarded as a model substance for the transition state in nucleophilic displacement at divalent chalcogen atoms, has been isolated and subjected to X-ray structure determination.
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    Zinc Complexes of Drugs Containing Nitrogen Heterocycles (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 779-785 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Drug ligands ; Captopril ; Isoniazid ; Nalidixic acid ; Mercaptopurine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Four drugs whose actions have a relation to the status of zinccontaining species in the human body were used as ligands in zinc complexes. Captopril (H2Cap) forms the compound [ZnCap] (1) presumed to be a coordination polymer with O and S coordination. Isoniazid, in the presence of zinc salts, is converted to 1,2-diisonicotinoyl hydrazide (H2Nih) which forms polymeric [Zn(Nih)NH3] (2) with trigonal-bipyramidal ZnO2N3 coordination. Nalidixic acid (HNal) and zinc perchlorate yield [Zn(HNal)2(H2O)2](ClO4)2 · 2 H2O (3) containing zinc in an octahedral ZnO6 environment. Mercaptopurine (H2Mer), in the presence of ammonia, forms [Zn(Mer)(NH3)2] . H2O (4) which is a coordination polymer containing tetrahedral ZnN4 units. The structures of [Zn(Nih)NH3], [Zn(HNal)2(H2O)2](ClO4)2 . 2 H2O, and [Zn(Mer)(NH3)2] . 2 H2O were determined diffractometrically.
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    Enantioselective Deprotonation of Benzyl Phosphates by Homochiral Lithium Amide Bases  -  Configurational Stability of Benzyl Carbanions with a Dialkoxyphosphoryloxy Substituent and Their Rearrangement to Optically Active α-Hydroxy Phosphonates (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 823-830 
    Details
    ISSN: 0009-2940
    Keywords: Phosphate-phosphonate rearrangement ; Carbanions, benzylic, configurational stability of ; Phosphonaes Lithium amides, homochiral ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Benzyl dialkyl phosphates are deprotonated enantioselectively by homochiral lithium amides of isopropyl(1-phenylethyl)amine or bis(1-phenylethyl)amine. The short-lived benzylic carbanions formed are virtually configurationally stable relative to the rearrangement to optically active phenyl-hydroxymethylphosphonates. The enantiomeric excesses are up to 50%. The pro-(S) hydrogen is removed by amides having (S) configuration. Homochiral diethyl (S)-phenyl[D1]-methyl phosphate [(S)-16c] is deprotonated by both LDA and n-BuLi with a high primary kinetic isotope effect (kH/D ≍ 50) and isomerizes to the corresponding α-hydroxy phosphonate with an enantiomeric excess of up to 85%.
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    Tris(1,10-phenanthroline)iron(II) Complexes  -  Broad Variation of the Redox Potential by 4,7-Substitution at the Phenanthroline Ligands[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 845-850 
    Details
    ISSN: 0009-2940
    Keywords: Phenanthroline synthesis ; Tris(phenanthroline)iron(II) complexes ; Redox potential ; Cyclic voltammetry ; Electron transfer, outer-sphere ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new 4,7-donor-substituted phenanthrolines 2a-h were synthesized and the corresponding tris(1,10-phenanthroline)iron(II) complexes 3a-h studied by cyclic voltammetry. In more detail three novel aza-crown ether-linked (phenanthroline)iron complexes were investigated, the redox potentials of which could be fine-tuned by the addition of group-Ia,IIa metal cations. All iron(II) complexes showed reversible waves at scan rates between 50 and 500 mV · s-1 and could be reversibly oxidized and reduced by chemical means.
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    Bis(cyclopentadienyl)methane-Bridged Dinuclear Complexes, 10Part 9: B. Stempfle, H. Werner, Gazz. Chim. Ital., 1995, 125, in press. The Bis(cyclopentadienyl)methane Link between Lewis Basic and Lewis Acidic Metal CentersDedicated to Prof. Dr. Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 877-881 
    Details
    ISSN: 0009-2940
    Keywords: Bis(cyclopentadienyl)methane ; Heterobimetallic complexes ; Imido complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mononuclear rhodium complexes [(C5H5CH2C5H4)-Rh(CO)2] (1) and [(C5H5CH2C5H4)Rh(PhC≡CPh)(PiPr3)] (2) readily react with nBuLi or TlOEt to yield the corresponding lithium salts 3 and 4 or thallium salts 5 and 6. The reaction of these salts with [(C5H5)Nb(NtBu)Cl2] (7) leads to the formation of the heterodinuclear compounds [{CH2(C5H4)2}-{Rh(CO)2}{(C5H5)Nb(NtBu)Cl}] (8) and [{CH2(C5H4)2}-{Rh(PhC≡CPh)(PiPr3)}{(C5H5)Nb(NtBu)Cl}] (9), respectively. Treatment of 3-6 with [Mo(NtBu)2Cl2] (10) gives the heterodinuclear Rh/Mo complexes [{CH2(C5H4)2}{Rh(CO)2}-{Mo(NtBu)2Cl}] (11) and [{CH2(C5H4)2}{Rh(PhC≡CPh)-(PiPr3)}{Mo(NtBu)2Cl}] (12). The analogous reaction of [Mo(NMes)2Cl2(DME)] (13) with 3-6 yields the corresponding complexes [{CH2(C5H4)2}{Rh(CO)2}{Mo(NMes)2Cl}] (14) and [{CH2(C5H4)2}{Rh(PhC≡CPh)(PiPr3)}{Mo(NMes)2Cl}] (15). From the monometallated ligand [(C5H5CH2C5H4)M] (M = Li: 16; M = Tl: 17) and the imidometal compounds 7, 10 and 13, the mononuclear complexes [(C5H5CH2C5H4)(C5H5)Nb-(NtBu)Cl] (18) and [(C5H5CH2C5H4)Mo(NR)2Cl] (R = tBu: 19; R = Mes: 20) have been obtained.
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    Addition von Hydrofullerid [C60H]- an koordinierte, ungesättigte Kohlenwasserstoffe: Bindung von Fulleren an Metallkomplexe über KohlenwasserstoffbrückenHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1059-1060 
    Details
    ISSN: 0009-2940
    Keywords: Fullerene ; Hydrofulleride ; Manganese complex ; Rhenium complex ; Iron complexes ; Ruthenium complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of Hydrofulleride [C60H]- to Coordinated, Unsaturated Hydrocarbons: Binding of Fullerene to Metal Complexes through Hydrocarbon BridgesHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet.Hydrofulleride [C60H]- is added to the hydrocarbon ligands of the cationic complexes [(OC)5Re(η2-C2H4)]+, [(OC)3Mn-(η6-C6H6)]+, [(OC)3M(η5-C6H7)]+ (M = Fe, Ru), [(OC)3Fe(η5-C7H9)]+, and [(η5-C5H5)Fe(η6-C5H4CH2)]+.
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    URL: http://dx.doi.org/10.1002/cber.19951281017
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    Controlled Conversion of the Transient 2-Mesityl-1,1-bis(trimethylsilyl)silene into a Tetrahydro-2,3-disilanaphthalene, a 1,2-Disilacyclobutane, or a 1,3-Disilacyclobutane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1083-1088 
    Details
    ISSN: 0009-2940
    Keywords: Silenes ; Silene dimerization ; 1,2-Disilacyclobutanes ; 1,3-Disilacyclobutanes ; 2,3-Disilanaphthalene, tetrahydro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mesityl[tris(trimethylsilyl)silyl]methanol (1) reacts with strong bases with elimination of trimethylsilanolate according to a Peterson-type mechanism, the outcome of the reaction being dependent on solvent, temperature, and nature of the organometallic base applied. Thus, 1 was converted by treatment with MeLi in ether at -78°C to (E)-1,2,3,8a-tetra -hydro-1-mesityl-5,7,8a-trimethyl-2,2,3,3-tetrakis (trimethylsi-lyl)-2,3-disilanaphthalene (3), formally a [2 + 4] cyclodimer of the transient silene (Me3Si)2Si=CHMes (2). The reaction of 1 with PhMgBr in THF after some days resulted in the formation of (Z)-3,4-dimesityl-1,1,2,2-tetrakis(trimethylsilyl) -1,2-disilacyclobutane (6) as the main product besides small quantities of 3, the polysilane (Me3SiSi(SiMe3)2CH2Mes (10), and the alkoxysilane (Me3Si)3SiCH(Mes)OSi(Si-Me3)2CH2Mes (7). Compound 6, the formal [2 + 2] cycloadduct of 2, can also be obtained by thermal treatment of 3 and is considered to be the thermodynamically more stable silene dimer whereas 3 is the kinetically preferred product. At high LiBr concentrations in the reaction mixture 1 was converted by PhMgBr in THF to (E)-2,4-dimesityl-1,1,3,3-tetrakis(tri- methylsilyl)-1,3-disilacyclobutane (13) besides 6 and [bis(tri-methylsilyl)silyl]mesityl(trimethylsiloxy)methane (11). The unforeseen formation of 13 is discussed as proceeding via the silene-lithium bromide adduct (Me3Si)2Si(Br)CH(Li)Mes (12). In the absence of LiBr 1 was converted by MeLi in THF at -78°C to 11 and the trisilane (Me3Si)2Si(Me)CH2Mes (4b). Probable pathways of the formation of all new compounds are discussed. For 6 and 13 the results of the X-ray structural analyses are given.
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    Metallkomplexe mit biologisch wichtigen Lisganden, LXXXLXXIX. Mitteilung: Lit.. (η3:η3-C10H16)Ru(IV)-Komplexe mit α-Aminocarboxylaten, α-Aminosäureestern und Peptidestern als Liganden (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1117-1125 
    Details
    ISSN: 0009-2940
    Keywords: 1,7-Dimethylocta-2,6-diene-1,8-diyl ; Ruthenium complexes ; α-Amino carboxylates ; α-Amino acid esters ; Peptide esters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes Containing Biologically Important Ligands, LXXXLXXIX. Mitteilung: Lit. .  -  (η3:η3-C10H16)Ru(IV) Complexes with α-Amino Carboxylates, α-Amino Acid Esters, and Peptide Esters as LigandsReactions of the chloro-bridged bis(allyl) complex [(η3:η3-C10H16)Ru(Cl)(μ-Cl)]2 with α-amino carboxylates and α-amino acid esters afford the complexes (η3:η3-C10H16)(Cl)RuNH2CHRCO2 (2) and (η3:η3-C10H16)(Cl)2-RuNH2CHRCO2R′ (3). Abstraction of chloride from 3 by Ag+ gives the N,O-chelates [(η3:η3-C10H16)(Cl)RuNH2CHRCO2R′]+BF4 (4). Cysteine methyl ester forms the N,S-chelate complex (η3:η3-C10H16)(Cl)RuNH2CH(CO2CH3)CH2S (5), and with histidine methyl ester a dinuclear complex 6 with N,N-histidine bridge is obtained. Compound 3d with L-PheOEt as ligand was characterized by X-ray diffraction.
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    [MeO(CH2CH2O)3(CH2)3C5Me4]FeCl: A Halfsandwich Iron (II) Chloride Complex of Remarkable Stability (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1135-1136 
    Details
    ISSN: 0009-2940
    Keywords: Hemilabile ligands ; Cyclopentadienyl ligands, functionalised ; Iron compounds ; Halfsandwich complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of iron(II) chloride with one equivalent of [MeO-(CH2CH2O)3(CH2)3C5Me4]Li in THF yields the title halfsand-wich complex 1, which is stable in solution up to room temperature. Compound 1 reacts with C5H5Li and CO to give [MeO(CH2CH2O)3(CH2)3C5Me4]Fe(C5H5) (2) and [MeO-(CH2CH2O)3(CH2)3C5Me4]Fe(CO)2CI (3), respectively, in high yields.
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    [Cp4Fe4(E2)2] Clusters with Triangulated Dodecahedral Fe4E4 Skeletons (E = P, As)Dedicated to Professor Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1145-1148 
    Details
    ISSN: 0009-2940
    Keywords: P2, As2, P2S2, and P2Se2 ligands ; Iron complexes ; Triangulated dodecahedra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermolysis of [CpFe(CO)2]2 (1) and P4 or As4 affords the iron clusters [Cp4Fe4(E2)2], E = As (2a), P (2b), the Fe4E4 skeleton of which consists of a triangulated dodecahedron. S8 and gray Se oxidize the P2 ligands of 2b with formation of [Cp4Fe4(P2X2)2], X = S (3a), Se (3b), complexes with the hitherto unknown P2X2 ligands, 2a, b and 3a, b have been characterized by X-ray crystallography.
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    Functionalized Diorganozinc Compounds: Key Reagents for the Synthesis of Enantiomerically Pure 2,5-Disubstituted cis- and trans-Tetrahydrofurans (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1021-1028 
    Details
    ISSN: 0009-2940
    Keywords: Synthesis, stereoselective ; Catalysis ; Tetrahydrofurans ; Dialkylzinc reagents ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,4-Diol derivatives 4a-i were synthesized stereoselectively by either reagent- or catalyst-controlled routes using the addition of functionalized diorganozinc reagents to aldehydes. The stereoselectivities along the reagent-controlled synthetic path were in the range between 80:20 and 95:5. The stereoselectivities along the catalyst route exceeded 95:5. The 1,4-diol derivatives 4 thus obtained were transformed into enantiomerically pure cis- and trans-2,5-disubstituted tetrahydrofurans (16-20) by means of an intramolecular Williamson reaction.
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    Contributions to the Chemistry of Boron, 231Part 230: Ref.. Synthesis and Structures of Borylated HydrazinesDedicated to Professor H. P. Fritz on the occasion of his 65th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1187-1194 
    Details
    ISSN: 0009-2940
    Keywords: Hydrazines ; N,N'-bis(diphenylboryl)-N,N'-dimethyl- ; N,N'-bis(diphenylboryl)-N',N'-dimethyl- ; N,N'-bis(dimethylphenylsilyl)- ; N,N'-bis(chloromesitylboryl)-N'-phenyl-N'-(trimethylsilyl)- ; 1,2,4,5,3,6-Tetrazadiborinane, 1,2,4,5-tetrakis(tert-butyldimethylsilyl)-3,6-difluoro- ; Triazadiborolidine, dihydro-, derivative ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The diboration of the diazene PhN = NSiMe3 (15) by diborane(4) derivatives provides a new synthetic route to N,N'-diborylated hydrazines. The product formed depends on the type of the diborane(4) compound. Thus, addition of dimesityldiboron dichloride to 15 in a 1:1 ratio afforded (mesCIB)PhN-N(SiMe3)(BClmes) (16) while bis(dimethyl-amino)diboron dichloride was found to react in a 1:2 ratio to give a triazadiborolidine derivative 17. In addition, it was demonstrated that in the solid state Me2N-N(BPh2)2 (8) is a derivative of a three-membered dihydroazadiboriridine C while its isomer, (Ph2B)MeN-NMe(BPh2) (7), forms no BN coordinative bond. The new 3,6-difluoro-1,2,4,5-tetraza-3,6-diborine 13 shows a twist conformation. The molecular structures of all these compounds were determined by X-ray crystal structure analysis, and the influence of the B substituent on the conformation is discussed.
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    Metal Complexes of Functional Isocyanides, XXV. Amino(hydrazino)carbene Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1061-1068 
    Details
    ISSN: 0009-2940
    Keywords: N-Isocyanides ; N-Isocyanodialkylamine complexes ; Carbene complexes ; Imaging-Plate data collection ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The N-isocyanodialkylamine metal complexes [M(CO)5CN-NR2] (M = Cr, W), trans-[MI2(CNNR2)2] (M = Pd, Pt), trans-[Pt(Cl)(CNNR2)(PPh3)2]BF4, and cis-[PtCl2(CNNR2)(PPh3)] [R = Et, iPr; 2 R = -{CHMe(CH2)3CHMe}-] react with primary amines to give the amino(hydrazino)carbene metal complexes [M(CO)5(C(NHR′)NHNR2}] (R′ = Me, nPr, Cy) (1-9), trans-[PtI2{C(NHMe)NHNR2}2] (10-12) and trans, and the amine adducts cis-[PtCl2{C(NHMe)NHNC(H)(Me) (CH2)3CHMe}(PPh3)] H2NMe (14), and trans-[PdI2{C (NHMe)NHNC(H)(Me)(CH2)3CHMe}2] 2 H2NMe (15). With secondary amines the amino(hydrazino)carbene metal complexes trans (18) and trans-[PtCl{C(NEt2)NHNEt2} (PPh3)2]BF4 (19) Were isolated. The complexes trans-[PtI2{C(NHCy)NHNiPr2}CNNiPr 2] (20) and trans-[PdI2 (NH2Cy){C(NHCy)NHNiPr2}] (21) were obtained by reaction of trans-[MI2(CNNiPr2)2] (M = Pd, Pt) with cyclohexylamine. The structures were assigned on the basis of IR, NMR- (1H, 13C, 31P), and mass spectroscopy as well as an X-ray structural analysis of 21.
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    Metallocenophanes, VIIPart VI: Ref.. Preparation and Characterisation of the Disilver(I) Complexes of Conjugated Polyenes with [2.2.2]Paracyclophanyl End Groups (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1079-1082 
    Details
    ISSN: 0009-2940
    Keywords: [2.2.2]Paracyclophanes ; Polyenes ; Silver complexes ; X-Ray structural analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of the disilver(I) complexes 3 and 4, polyene metal complexes that are terminally substituted with [2.2.2]paracyclophanyl units, is described. NMR spectro-scopic studies on the disilver perchlorate complex 3b showed that (a) the sites of complexation are the cyclophane groups and (b) the olefinic spacers do not overly perturb the overall complexation properties of the individual [2.2.2]paracyclo-phanyl groups. The crystal structures of the disilver hexafluo-roantimonate complexes 4a-b were determined. The use of the hexafluoroantimonate counterion and solvent mixtures containing toluene both proved crucial in obtaining single crystals; toluene is incorportated into the crystal lattices.
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    Highly Substituted Tris(pyrazolyl)methane Ligands and Some Zinc Complexes Thereof (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1095-1103 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Tridentate ligands ; Tris(pyrazolyl)methane ; Reactivity ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(pyrazolyl)methane ligands in which two or three of the pyrazole carbon atoms bear organic substituents (L1-L7) were synthesized from chloroform and the corresponding pyrazole under phase transfer conditions. Their behavior towards zinc salts was found to span the range from no reaction at all to hydrolytic destruction. One hydrolysis product isolated and structurally characterized was the perchlorate complex [(HPz5)3Zn-OClO3]ClO4 (1), other ones were the 2:1 complexes (HPz3)2ZnBr2 (2) and (HPz6)2Zn(NO3)2 (3, HPzn = substituted pyrazole). Zinc perchlorate and tris(trimethylpy-razolyl)methane (L2) formed the octahedral binary complex [L22Zn](ClO4)2 (4) as evidenced by a structure determination. Zinc halides produced the 1:1 complexes L1 · ZnBr2 (5), L4 · ZnCl2 (6), and L4 · ZnBr2 (7), which according to the structure determinations of 6 and 7 contain tetrahedral ZnN2Hal2 units with only bidentate tris(pyrazolyl)methane ligands. In contrast, the zinc nitrate complex L4 · Zn(NO3)2 (8) was found to have an octahedral structure with mono- and bidentate nitrate and tridentate L4. The bromide complex 7 was converted by silver perchlorate hydrate into the labile compound [L4 · ZnBr]ClO4 (9) and then into the unstable product [L4 · Zn-OH2](ClO4)2 (10), both presumed to contain zinc in a tetrahedral ZnN3Br or ZnN3O environment, respectively. The ease of hydrolytic self-destruction prevented the exploitation of the reactivity of 9 and 10 in analogy to that of the corresponding tris(pyrazolyl)borate zinc complexes.
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    Unusual Complexation Behavior of Metallomacrocycles Based on Isothiosemicarbazides with Respect to Alkali and Alkaline Earth Metal Ions: Novel 2:1 Associates (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1089-1093 
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    ISSN: 0009-2940
    Keywords: Metallomacrocycles ; Nickel complexes ; Complexation reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions between alkali and alkaline earth metal ions and nickel(II) macrocycles based on S-alkylated isothiosemi-carbazides with different crown ether cavity size were studied in propylene carbonate by spectrophotometric and calorimetric titrations. Metallomacrocycles 1 and 2 exhibit normal behavior on 1:1 complexation with alkali- and alkaline earth metal ions and resemble in this respect 15C5 and 18C6, respectively. The most stable complexes are formed by these “ligands” when the diameter of the cation and the crown ether hole have approximately the same size. The most striking feature of the complexation processes studied is the formation of 1:2 metal-ligand associates even in the case of the smallest cations. These associates are very different from “normal” crown ether sandwich complexes. In reality, the particle formed is an associate between a 1:1 complex, in which the corresponding metal ion is well accommdated inside the ligand cavity, and a second metallomacrocyclic ligand. Their formation is disfavored by enthalpic contributions. A special kind of “switch” from these associates to normal sandwich complexes takes place in the case of 1, when the cation diameter compared to hole size increases. The macrocycle 2 forms this kind of associates with all akali and alkaline earth ions.
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    Synthesis and Reactivity of Silicon Transition Metal Complexes, 3433. Mitteilung: Lit.. Pentachlordisilanyl- und Disilanyl-Komplexe von Molybdän und Wolfram: Darstellung, Struktur und spektroskopische CharakterisierungHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1109-1115 
    Details
    ISSN: 0009-2940
    Keywords: Silicon transition metal complexes ; Metallodisilanes ; Nucleophilic metallation ; Cl/H exchange at silicon ; Raman spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactivity of Silicon Transition Metal Complexes, 34[*].  -  Pentachlorodisilanyl and Disilanyl Complexes of Molybdenum and Tungsten: Synthesis, Structure, and Spectroscopic CharacterizationReaction of the lithium metallates Li[M(PMe3)(CO)2C5R5] [M = Mo, W; R = H (1a, b), Me (1c, d)] with Si2Cl6 (2) leads to the formation of the pentachloro(metallo)disilanes 5R5(OC)2(Me3P)M - SiCl2 - SiCl3 (3a - d), which are transformed into the metallo disilanes C5R5(OC)2(Me3P)M - SiH2 - SiH3 (4a - d) on treatment with LiAlH4. The disilanes 4a - d are reconverted into 3a - d in the presence of tetrachloromethane. Extensive spectroscopic investigations (NMR, Raman, and IR spectroscopy) were performed to establish the transition-metal effect especially with respect to the H5Si2 ligand. The molecular structure of C5Me5(OC)2(Me3P)W - SiCl2 - SiCl3 (3d) was determined by single-crystal X-ray diffraction.
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    Octacarbonylbis {μ-(tris(trimethylsilyl)methyl]indany l} dimanganese with Two Monoalkyl Indium Groups Bridging the Mn-Mn Bond (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1137-1139 
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    ISSN: 0009-2940
    Keywords: Tetraindane(4) ; Indium(I) ; Mn-Mn bond ; Indium alkyl bridge ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetrahedra-tetrakis[tris(trimethylsilyl)methyl]tetraindane(4) (1) reacts with decacarbonyldimanganese(0) to yield the bright red crystalline title compound 2, in which two carbonyl ligands are replaced by two InR fragments. The crystal structure determination of 2 shows two Mn(CO)4 groups (Mn-Mn 313.7 pm) bridged by two monoalkylindium units and a planar Mn2In2 molecular center.
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    Thioselonocarboxylic Ester, Selenetane, and Dihydrodiselenine Complexes Prepared from Pentacarbonyl(selenobenzaldehyde)tungsten with π-Donor-Substituted Alkynes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1149-1156 
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    ISSN: 0009-2940
    Keywords: Selenoaldehyde complex ; Thioselonocarboxylic ester complexes ; Selenetane complex ; Dihydrodiselenine complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyltungsten-coordinated selenobenzaldehyde, [(CO)5W{Se=C(Ph)H}] (1), reacts with tBu-C≡C-SMe (2) by insertion of the C≡C into the Se=C bond to form in a highly regio- and stereoselective manner the α,β-unsaturated thioselonocarboxylic ester complex (Z)(C=C)-[(CO)5W{≡1-Se=C(SMe)C(tBu)=C(Ph)H}] (3). The thioselonocarboxylic ester ligand is cleaved intact from the metal by treatment of 3 with [NEt4]Br. Three complexes are formed in the reaction of 1 with Me-C≡C-SMe (5): the thioselonocarboxylic ester complex [(CO)5W{≡1-Se=C(SMe)C(Me)=C(Ph)H}] (6) as a mixture of the (E) and (Z)(C=C) isomers, a selenetane complex (7) and a dihydrodiselenine complex (8). The product distribution depends on the ratio 1:5 and on the solvent. The reaction of 1 with the bis(organylthio)alkynes RS-C≡C-SR (9) [R = Me (a), iPr (b), 2,6-C6H3Me2 (c)] yields mixtures of the (E) and (Z)(C=C) isomers of the α,β-unsaturated α-organylthio thioselonocarboxylic ester complexes [(CO)5W{≡1-Se=C(SR)C(SR)=C(Ph)H)] (10a-c). In contrast, the reaction of 1 with tert-butoxyethyne, H-C≡C-OtBu (11), affords a bis(pentacarbonyltungsten) 5,6-dihydro-1,2-diselenine complex (12). Compound 12 is probably formed by consecutive reaction of 1 with 11 to give the selonocarboxylic ester complex [(CO)5W{≡1-Se=C(OtBu)C(H)=C(Ph)H}] which then further reacts as a heterodiene by highly regioselective [4 + 2] cycloaddition with the Se=C bond of a second molecule of 1 to give 12. In the reaction of 1 with 5 and 9a the isomer with a trans arrangement of C(=Se)SMe and Ph is the kinetically controlled reaction product [(E)-6 and (Z)-10a, respectively]. The formation of (E)-6 and (Z)-10a is followed by isomerization until an (E)/(Z) equilibrium is reached. Complexes 3 and 7 were characterized by X-ray structural analyses.
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    Tin for Organic Synthesis, 13Part 12: Ref.. A New and Regioselective Method for the Synthesis of Aromatic, Heteroaromatic, and Olefinic Sulfonamides by Electrophilic Destannylation (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1195-1198 
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    ISSN: 0009-2940
    Keywords: Electrophilic aromatic substitution ; Electrophilic vinylic substitution ; Trialkylstannanes, application of ; Sulfonamides, synthesis of ; Sulfodestannylation, application of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A mild and effective method for the preparation of aromatic and olefinic sulfonamides is described. The reaction of trialkylaryl- (4a-f), heteroaryl- (4g), and vinylic stannanes (4h) with sulfuryl chloride and secondary amines provides the corresponding sulfonamides in an ipso-specific manner.
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    Ylidylphosphorsulfide, -selenide, -disulfide, -sulfidselenide und -diselenide (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1207-1219 
    Details
    ISSN: 0009-2940
    Keywords: Ylide-substituted phosphorus ; Phosphorus sulfides ; Phosphorus selenides ; Thioxophosphanes ; Selenoxo-phosphanes ; Dithioxophosphoranes ; Diselenoxophosphoranes ; Alkylation reactions ; Selenadiphosphirane ; 2,5,7-Triselena-1,3,4,6-tetraphosphanorbornane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ylidylphosphorus Sulfides, Selenides, Disulfides, Sulfide Selenides, and DiselenidesWe report on the first stable monomeric phosphorus mono-chalcogenides 2, 8 and the first stable dichalcogenides 4, 10 without bulky or intramolecularly coordinating substituents. They are stabilized by a high contribution of the zwitterionic resonance formula, which follows both from the NMR spectra and from an X-ray structure determination. Their preparation starts from triphenylphosphoniumylidyl-dichlorophosphanes 1. For the monochalcogenides they are treated with sodium sulfide or selenide or better with bis(trimethylsilyl) sulfide or selenide. In case of the C-phenyl and C-meta-tolyl representatives and also of the C-trimethylsilyl compound a number of secondary, partly novel products are obtained. - The dichalcogenides result from the reaction with sodium disulfide and diselenide, respectively, or from the oxidation of the monochalcogenides. - Alkylation of the monochalcogenides results in ylidylalkylchalcogenophosphenium salts 13, 15. In solution they are in equilibrium with more or less of the covalent form 14, 16, depending on the anion and on the solvent. Alkylation is often accompanied by secondary reactions. A diselenide loses selenium on alkylation.
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    Synthesis and Reactivity of Silicon Transition Metal Complexes, 3332. Mitteilung: Lit.. Metallo Silanols and Metallo Siloxanes, 87. Mitteilung: Lit.. Metallo-silanole vom Typ C5R5(OC)2(Me3P)M - SiPh2OH (M = Cr, Mo, W): Darstellung nach der Dimethyldioxiran-Methode und Überführung in funktionalisierte Metallo-disiloxaneHerrn Professor Max Schmidt zum 70. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1251-1255 
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    ISSN: 0009-2940
    Keywords: Oxofunctionalization ; Dimethyldioxirane ; Metallo silanes ; Metallo silanols ; Metallo siloxanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactivity of Silicon Transition Metal Complexes, 3332. Mitteilung: Lit. .  -  Metallo Silanols and Metallo Siloxanes, 8 7. Mitteilung: Lit. .  -  Metallo Silanols of the Type C5R5(OC)2(Me3P)M-SiPh2OH (M = Cr, Mo, W): Preparation According to the Dimethyldioxirane Route and Conversion into Metallo Disiloxanes Herrn Professor Max Schmidt zum 70. Geburtstag gewidmet.The metallo silanes C5R5(OC)2(Me3P)M-SiPh2H (4a-c), are converted into the corresponding metallo silanols C5R5(OC)2-(Me3P)M-SiPh2OH [R = H, M = Cr (6a); R = Me, M = Mo (6b); M = W (6c)] by oxofunctionalization with dimethyldioxirane (5). Treatment of 6b, c with the chlorosilanes Me2Si(R)Cl [R = H (3b), [R = Cl (3c)] in the presence of triethylamine gives access to the metallo disiloxanes C5Me5(OC)2(Me3P)M-SiPh2OSiMe2R (M = Mo, R = H (7a); M = W, R = Cl (7b)]. The structure of tungsten silanol 6c is determined by X-ray diffraction analysis.
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    Synthesis and Characterization of β-Phosphaenones An Investigation on the Conjugative Properties of the P=C Bond (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 465-476 
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    ISSN: 0009-2940
    Keywords: Phosphaalkenes, C-halo, C-metal ; Phosphaacrylic acid ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermally and air-stable β-phosphaenones were synthesized by functionalization of Mes*P=CCl2 (1; Mes* = supermesityl = 2,4,6-tri-tert-butylphenyl). At low temperature, 1 was lithiated by halogen-metal exchange with n-butyllithium to give the phosphanylidene carbenoid (Z)-Mes*P=C(Cl)Li [(Z)-2] which reacted with acid chlorides to furnish the C-carbonyl-substituted phosphaalkenes (Z)-Mes*P=C(Cl)R (3: P = COtBu; 4: R = COPh; 5: R = COOEt). The reaction of (Z)-2 with carbon dioxide furnished the carboxylate 6, which was converted by treatment with pivaloyl chloride or trimethylsilyl chloride into the phosphaalkenes 7 and 8 functionalized at the carbon atom by an anhydride or a trimethylsilyl ester function, respectively. Acidification of 6 or hydrolysis of 8 with water in chloroform solution afforded the novel carboxylic acid (Z)-Mes*P=C(Cl)COOH (9). Spectroscopic investigations (NMR, UV, IR) of 3-9 and the X-ray structures of 3 and 4 are presented. Based on these properties and on theoretical calculations, the occurrence of conjugation in the β-phosphaenone system is discussed and compared with the well-known conjugation in normal enones.
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    Reactions of Phosphaalkenes with HexafluoroacetoneDedicated to Professor H. M. R. Hoffmann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 499-502 
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    ISSN: 0009-2940
    Keywords: Phosphaalkenes ; Cycloadditions ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dimethylamino-substituted phosphaalkene 1 reacts with hexafluoroacetone (HFA) with addition at the P=C bond to form the 1,5,2-dioxaphosphorinane 2. The structure of 2 was confirmed by an X-ray crystal structure analysis. The six-membered ring displays an envelope conformation with the phosphorus atom out of the plane, but the phosphorus is disordered over two sites. Reaction of P-trimethylsilyl-substituted phosphaalkenes with HFA proceeds with retention of the P=C double bond and insertion of HFA into the P—Si bond. Two isomeric products are obtained and are characterized by 1H-, 13C-, 19F-, and 31P-NMR spectroscopy, IR spectroscopy, mass spectrometry, and elemental analysis.
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    Monomere (Acetylacetonato)kupfer(I)-Komplexe von Alkinen und 1,4-Diinen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 525-529 
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    ISSN: 0009-2940
    Keywords: Copper complexes ; Acetylacetonate ; Alkynes ; 1,4-Diynes ; Titanocenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monomeric (Acetylacetonato)copper(I) Complexes of Alkynes and 1,4-DiynesMonomeric (η2-Me3SiC≡CSiMe3)Cu(acac) (3) is formed by the reaction of dimeric [(η2-Me3SiC≡CSiMe3)CuBr]2 (1) with two equivalents of Na(acac) (2). In a similar manner Me2-Si(C≡CSiMe3)2 (4) reacts with CuCl (5) and 2 to afford Me2Si[(η2-C≡CSiMe3)Cu(acac)]2 (6). In compounds 3 and 6 an alkyne unit is η2-coordinated to a monomeric Cu(acac) moiety with a copper atom in a planar environment. With the organometallic 1,4-diyne (η5-C5H4SiMe3)2Ti(C≡CSiMe3)2 (7), compound [(η5-C5H4SiMe3)2Ti(C≡CSiMe3)2]Cu(acac) (8) is formed. In 8 both Me3SiC≡C ligands of the 3-titanapenta-1,4-diyne fragment are η2-coordinated to a monomeric Cu-(acac) building block. The copper atom in 8 possesses a pseudo-tetrahedral environment (shown by X-ray analysis), built by the two Me3SiC≡C ligands of the (η5-C5H4SiMe3)2-Ti(C≡CSiMe3)2 moiety and the two oxygen atoms of the acetylacetonato ligand. 8 is additionally formed by the reaction of 3 or 6 with 7, or by treatment of [(η5-C5H4SiMe3)2Ti(C≡C-SiMe3)2]CuCl (9) with Na(acac) (2). The application of 3, 6, and 8 as precursors for the preparation of copper films in the CVD process of copper(I) is discussed.
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    Chiral Organometallic Reagents, XIIIPart XII: Ref.. Structural Aspects of Differentially Solvated Benzyllithium Contact Ion Pairs (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 551-556 
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    ISSN: 0009-2940
    Keywords: Benzyllithium compounds ; Ion pairs ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The solvation and ion pair nature of α-(phenylthio)benzyllithium (2d) in THF solution were investigated by NMR-spectroscopic methods. The effect of additives such as diethylene-glycol dimethyl ether or of 12-crown-4 was studied. The results were compared to those of benzyllithium compounds 4 and 6, containing a pentaoxapentadecane ansa chain. These compounds exist as contact ion pairs in which lithium is held at the anionic carbon. This is reflected in the 6Li,13C coupling and 1H,6Li-HOESY contacts in the NMR spectra.
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    Sulfur Compounds, Part 186Part 185: K. Bergemann, M. Kustos, P. Krüger, R. Steudel, Angew. Chem., in print.. The Synthesis of Cyclic Organosulfur Compounds from (C5H5)4Ti2C2S4 by Ligand Transfer Reactions (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 561-564 
    Details
    ISSN: 0009-2940
    Keywords: Titanocene complexes ; Organosulfur ligands ; Ligand transfer ; Organosulfur heterocycles ; Sulfur-sulfur bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tetrathiaoxalate complex Cp4Ti2C2S4 (1) reacts with an equimolar amount of COCl2 to give the blue-green mononuclear complex Cp2TiC2S4CO (4). This reaction is analogous to the known reactions of 1 with SCl2 or S2Cl2. However, when 1 was treated with equimolar amounts of the bifunctional sulfenyl chlorides 1,2-C2H4(SCl)2 (5), 1,3-C3H6(SCl)2 (6) or 1,2-C6H4(SCl)2 (7), the bi- or monocyclic tetrakisdisulfanes C6H8S8 (9b), C8H12S8 (10), and C14H8S8 (11), respectively, were obtained. The X-ray crystal structure analysis of 11 · CS2 showed that 11 possesses Ci symmetry with a central exocyclic CC double bond similar to tetrathiafulvalenes: C6H4(μ-S2)2C=C(μ-S2)2C6H4.
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    Norbornadiene(bipyridyl)molybdenum(II) Complexes: Synthesis, Structure and Reactivity of [Mo(CO)(C7H8)(C10H6R2N2)X2] (X = I, Br)Dedicated to Professor Dr. Helmut Werner on the occasion of his birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1007-1013 
    Details
    ISSN: 0009-2940
    Keywords: Tetracarbonyl(norbornadiene)molybdenum(0) ; Oxidative addition of I2 ; Dihalogeno(bipyridyl)molybdenum(II) complexes ; 7-Coordinated complexes ; Neutral and cationic molybdenum(II) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of [Mo(CO)4(C7H8)] (1) with I2 gave the norbornadienemolybdenum(II) complex [Mo(CO)2(C7H8)I2]n≥1 (2), which existed in an equilibrium of two isomeric forms. In acetonitrile, 2 reversibly formed the adduct [Mo(CO)2-(C7H8)(NCCH3)I2] (3), whereas on treatment with 2,2′-bipyridine or 4,4′-di-2,2′-tBu-bipyridine, it gave stable 7-coordinated molybdenum(II) complexes, [Mo(CO)(C7H8)-(C10H8N2)I2] (4) and [Mo(CO)(C7H8)(C10H6tBu2N2)I2] (5), in good yield. In similar reactions, the related dibromomolybdenum compounds [Mo(CO)(C7H8)(C10H8N2)Br2] (6) and [Mo-(CO)(C7H8)(C10H6tBu2N2)Br2] (7) were prepared by oxidation of 1 with two equivalents of CuBr2. The X-ray structural analysis of 6 reveals that the geometry around the molybdenum atom is nearly perfectly pentagonal bipyramidal, with the CO and one of the bipyridyl rings perpendicular to the plane formed by the other ligands. The compounds 5 and 6 react with AgSbF6 by halogen abstraction to give cationic complexes, {[Mo(CO)(C7H8)(C10H8N2)Br]SbF6}n≥1 (8) and {[Mo(CO)(C7H8)(C10H6tBu2N2)I]SbF6}n≥1 (9): In acetone, 8 and 9 reversibly formed the adducts [Mo(CO)(C7H8)(C10H8N2)(acetone)Br]SbF6 (8′) and [Mo(CO)(C7H8)(C10H6tBu2N2)(acetone)I]SbF6 (9′); while on treatment with PMe3, the stable monomeric complexes, [Mo(CO)(C7H8)(C10H8N2)(PMe3)Br]SbF6 (10) and [Mo(CO)(C7H8)(C10H6tBu2N2)(PMe3)I]SbF6 (11), were isolated in almost quantitative yield. In the presence of KBr, compound 8′ reverted to the dibromo complex 6, whereas 9′ reacted to produce a 1:1:2 mixture of 5, 7 and the bromo(iodo) complex [Mo(CO)(C7H8)(C10H6tBu2N2)BrI] (12). The same mixture is available from the reaction of 5 with one equivalent of 7.
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    Graphical Abstract (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. A149 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951281018
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    Amino Substituted Tricarbonyl(cyclobutadiene)iron Complexes: Pd-Catalyzed Coupling of Iodocyclobutadiene Complexes with Amines (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1055-1058 
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    ISSN: 0009-2940
    Keywords: Aminations ; Palladium catalysis ; Organometallic amines ; Coupling reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coupling of the iodides 1 with amines under palladium catalysis affords the novel aminated cyclobutadiene derivatives 2 in preparative useful yields.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951281101
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    Chiral Carbanions, 1. Configurational Stability and Reactions of α-Acyloxy-Substituted α-Methylbenzyllithium Compounds (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1069-1077 
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    ISSN: 0009-2940
    Keywords: Esters, 1-phenylethyl ; Carbanions, α-methyl-α-oxybenzyl, Configurational stability ; Ester - hydroxy ketone rearrangement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Racemic and optically active 1-phenylethyl esters of pivalic, ( - )-camphanic and 2,4,6-triisopropylbenzoic acid were prepared. The esters 7a of pivalic acid were deprotonated with lithium 2,2,6,6-tetramethylpiperidide (Li-TMP) to form α-oxy-α-methylbenzyllithium compounds which are partly con-figurationally stable prior to acylation with starting material. Camphanic ester (-)-7b cannot be deprotonated by Li-TMP and tBuLi is added to the ester function to afford ketone (-)-12a. 1-Phenylethyl 2,4,6-triisopropylbenzoates 16 were transformed within minutes to carbanions 19 by using sBuLi/TMEDA in THF, hexane, toluene and sBuLi without TMEDA in toluene/20% diethyl ether at -78°C. The carbanions are configurationally stable only in toluene/20% diethyl ether and racemise partly in the other solvents. They react with a variety of electrophiles with either retention [MeOD, AcOD, (MeO)2CO, CICO2Me] or inversion (Me3SnCl) of configuration. Carbanions 19 rearrange on warming to -20°C to hydroxy ketone 24 with racemisation.
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    Metal Complexes with Tetrapyrrole Ligands, LXIX. Facile Synthesis and 13C-NMR Spectrum of Dichloro(octaethylporphyrinato)zirconium(IV) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1131-1133 
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    ISSN: 0009-2940
    Keywords: Zirconium(IV) octaethylporphyrin complex ; Dichlorozirconium(IV) porphyrin complex ; Precursor of organometallic compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of dichloro(2,3,7,8,12,13,17,18-octaethylpor-phyrinato)zirconium(IV), Zr(oep)Cl2, from zirconium tetrachloride and octaethylporphyrin, H2(oep), is described. The reported synthesis is a new and simple route to this precursor of organometallic compounds. Zr(oep)Cl2 was characterized by elemental analyses, 1H- and 13C-NMR, UV/Vis, and mass spectra. Hydrolysis yielded a mixture of mono- and binuclear hydroxy zirconium(IV) porphyrins.
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    URL: http://dx.doi.org/10.1002/cber.19951281112
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    Stereochemie aliphatischer Carbokationen, 13. Protonierte Cyclopropane als Zwischenstufen von 1,2-Alkylverschiebungen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 129-141 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Stereochemistry of Aliphatic Carbocations, 13. Protonated Cyclopropanes as Intermediates in 1,2-Alkyl ShiftsThe nitrous acid deamination of 2-ethyl-1-methylbutylamine (10), 1,2-diethylbutylamine (35), and 2-ethyl-1-methylpentylamine (43) has been studied with respect to 1,2-alkyl shifts. Optically active and deuterated amines were employed whenever possible. The structure, configuration, and deuterium distribution of various products (e.g. 16 from 10, 40 and 48 from 35, 56 from 43) are most reasonably explained in terms of alkyl-bridged intermediates (corner-protonated cyclopropanes) which isomerize via proton shifts from corner to corner. The alternative interconversion of open ions via 1,3-H shifts is incompatible with our experimental results.
    Notes: Die Desaminierung von 2-Ethyl-1-methylbutylamin (10), 1,2-Diethylbutylamin (35) und 2-Ethyl-1-methylpentylamin (43) mit salpetriger Säure wurde im Hinblick auf 1,2-Alkylverschiebungen untersucht. Soweit möglich wurden optisch aktive und deuterium-markierte Amine eingesetzt. Die Struktur, Konfiguration und Deuterium-Verteilung verschiedener Produkte (z.B. 16 aus 10, 40 und 48 aus 35, 56 aus 43) wird am besten erklärt mit Hilfe alkylverbrückter Zwischenstufen (eckenprotonierter Cyclopropane), die durch Protonenverschiebung von Ecke zu Ecke isomerisieren. Die alternative Umwandlung offener Kationen durch 1,3-H-Verschiebung ist mit unseren experimentellen Ergebnissen unvereinbar.
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    Kristall- und Molekülstrukturen des S3N2+-Radikalkations in S3N2+SO3CF3- · 1/2 CH3CN und von S3N2(NSO2F) (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 226-232 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structures of the S3N2+ Radical Cation in S3N2+SO3CF3- · 1/2 CH3CN and of S3N2(NSO2F)The molecular and crystal structures of S3N2+SO3CF3- · 1/2 CH3CN (1) and S3N2NSO2F (2) were determined from single crystal X-ray diffraction data. The S3N2+ radical cation in 1 is planar, two cations being connected through weak S—S bonding interactions to form dimers with a chair configuration. The S3N2 ring of 2, in which the NSO2F group is covalently bonded to one of the S atoms of the S — S group, is not planar; the S — S bond is weaker than in 1.
    Notes: Die Röntgenstrukturanalysen von S3N2+SO3CF3- - 1/2 CH3CN (1) und S3N2NSO2F (2) zeigen in 1 ein planares S3N2+-Radikalkation, wobei zwei Kationen über schwache S-S-Wechselwirkungen zu sesselförmigen Dimeren assoziiert sind. Der an einem S-Atom der S — S-Gruppe substituierte S3N2-Ring in 2 ist nicht planar; die S — S-Bindung ist schwächer als in 1.
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    Kinetische und mechanistische Untersuchungen von Übergangsmetallkomplex-Reaktionen, IV. Reaktionen von Komplexliganden, XVIII. Kinetik und Mechanismus der Einschiebung von 1-(Diethylamino)-1-propin in die Metall-Carbenkohlenstoff-Bindung von Pentacarbonyl(arylmethoxycarben)chrom(O) und -wolfram(O) (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 193-202 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kinetic and Mechanistic Investigations of Transition Metal Complex Reactions, IV. Reactions of Complex Ligands, XVIII. Kinetic and Mechanism of the Insertion of 1-(Diethylamino)-1-propyne into the Metal-Carbene Bond of Pentacarbonyl(arylmethoxycarbene)chromium(0) and -tungsten(0)Pentacarbonyl(arylmethoxycarbene) complexes (CO)5M[C(p-C6H4R)OCH3] (M = Cr, W; R = CF3, Br, H, CH3, OCH3) (1a - g) add 1-(diethylamino)-1-propyne (2) via insertion of the alkyne into the metal-carbene bond. The formation of pentacarbonyl[(diethylamino)(2-aryl-2-methoxy-1-methylethenyl)carbene]chromium(0) and -tungsten(0) (3a - g) in octane follows a second-order rate law: d[3]/dt = k[1][2]. The tungsten complexes react faster than the analogous chromium compounds. Replacement of R = H by electron withdrawing substituents (CF3, Br) results in an increase, by electron donating groups (CH3, OCH3) in a decrease of the reaction rate. The activation enthalpies ΔH≠ are low (25.1 - 39.4 kJ · mol-1), the activation entropies ΔS≠ strongly negative (-129 to -145 J · mol- K-1). The results are discussed on the basis of an associative stepwise mechanism with an attack of the ynamine at the carbene carbon in the first reaction step.
    Notes: Pentacarbonyl(arylmethoxycarben)-Komplexe (CO)5M[C(p-C6H4R)OCH3] (M = Cr, W; R = CF3, Br, H, CH3, OCH3) (1a - g) addieren 1-(Diethylamino)-1-propin (2) unter Einschiebung des Alkins in die Metall-Carbenkohlenstoff-Bindung. Die Bildung von Pentacarbonyl[(diethylamino)(2-aryl-2-methoxy-1-methylethenyl)carben]chrom(0) und -wolfram(0) (3a - g) in Octan erfolgt nach einem Geschwindigkeitsgesetz zweiter Ordnung: d[3]/dt = k[1][2]. Die Wolframkomplexe reagieren schneller als die entsprechenden Chromverbindungen. Ersatz von R = H durch elektronenziehende Substituenten (Br, CF3) führt zu einer Erhöhung, durch elektronenspendende Gruppen (CH3, OCH3) zu einer Verringerung der Reaktionsgeschwindigkeit. Die Aktivierungsenthalpien ΔH≠ sind niedrig (25.1 - 39.4 kJ · mol-1), die Aktivierungsentropien ΔS≠ stark negativ (-129 bis -145 Jmol-1 K-1). Die Ergebnisse werden auf der Grundlage eines mehrstufigen Mechanismus mit einem Angriff des Inamins am Carbenkohlenstoff im ersten Reaktionsschritt diskutiert.
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    Sugar enolones, XII. Peroxidation of pyranose-derived enol esters: An efficacious synthesis of peracetylhexosuloses and their conversion into γ-pyrones via 3,2-enolones (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 489-510 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zucker-enolone, XII. Peroxidation pyranoider Enolester: Eine ergiebige Synthese von Peracetyl-hexosulosen und ihre Umwandlung in γ-Pyrone über 3,2-EnoloneVon Pyranosen abgeleitete 1,2-Enolacetate des Typs 4 reagieren mit 3-Chlorperbenzoesäure in Ether glatt zu einem Gemisch anomerer Glycos-2-ulose-acetate 6, wie anhand der Umwandlungen 7 → 11/12, 18 → 19/20 und 21 → 22 gezeigt wird. Konstitution und Konfiguration der Produkte stützen sich auf NMR-Daten, auf die Charakterisierung von Hydrierungsprodukten (10 bzw. 23) sowie im Falle von 11, 12 und 22 auf deren Bildung aus den entsprechenden partiell acetylierten Pyranosen 8, 9 und 23 durch RuO4-Oxidation. - Saure Acetylierung überführt die Glycos-2-ulosen in ihre 2,2-Diacetoxy-Derivate (13, 24 bzw. 35) unter Anomerisierung der β-Isomeren; bei vorsichtiger Behandlung mit Acetylchlorid/Pyridin werden dagegen, unter Erhalt der Konfiguration an C-1, die peracetylierten 2,3-Dehydro-pyranosen 15, 17 und 36 erhalten. Unter schwach basischen Bedingungen erfolgt die Ausbildung des γ-Pyron-Systems (42/43) durch doppelte Eliminierung von Essigsäure, wobei die Zwischenprodukte isolierbar sind und als die 3,2-Enolone 37α, 37β und 38 charakterisiert werden können. Hierbei konnte das aus der Tetraacetyl-glucose 44 durch Oxidation leicht darstellbare Triacetyl-endiolon 41, das Zwischenprodukt des Übergangs 11 → 42 sein soll40, als Intermediat ausgeschlossen werden.
    Notes: Pyranose-derived 1,2-enol acetates of type 4 readily react with 3-chloroperbenzoic acid in ether to an anomeric mixture of glycos-2-uloses 6, as is demonstrated by the conversions 7 → 11/12, 18 → 19/20 and 21 → 22. Structural and configurational assignments were based on NMR-data, on the characterization of hydrogenation products (10 and 23), and on the independent formation of 11, 12, and 22 by RuO4-oxidation of the respective partially acetylated pyranoses 8, 9, and 23. -Acid-catalyzed acetylation converts the glycos-2-uloses into their 2,2-diacetoxy derivatives (13, 24, and 35) with anomerization of β-isomers, whereas cautious treatment with acetyl chloride/pyridine affords the peracetylated 2,3-dehydropyranoses 15, 17, and 36 with retention of configuration at C-1. Mildly basic conditions initiate the elaboration of the γ-pyrone systems (42/43) via double elimination of acetic acid, the respective intermediates, 3,2-enolones 37α, 37β, and 38, being readily isolable. The alternate triacetyl-enediolone 41, allegedly40 an intermediate in the conversion 11 → 42 could be excluded as an intermediate on the basis of its synthesis from tetraacetyl-glucose by oxidation and elimination of acetic acid (44 → 45 → 41).
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    Alkine und Cumulene, XII. Über die Verwendung von Acetylendicarbonsäure-di-tert-butylester in Diels-Alder-Additionen (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 531-541 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Alkynes and Cumulenes, XII. The Application of Di-tert-butyl Acetylenedicarboxylate in Diels-Alder AdditionsDi-tert-butyl acetylenedicarboxylate (1) may be added in good yields to the model dienes 1,3-butadiene (6a), 2-methyl-1,3-butadiene (6b), 2,3-dimethyl-1,3-butadiene (6c), furan (10), and 1,3-cyclohexadiene (19) to afford the Diels-Alder adducts 7a - c, 12 (E = CO2C(CH3)3), and 20, respectively. Under certain conditions the reaction with 10 also leads to the four 2:1-adducts 13 - 16 (E = CO2C(CH3)3). Whereas the esters 7a - c are converted in quantitative yields to the corresponding anhydrides 8a - c by warming in the presence of catalytic amounts of p-toluenesulfonic acid or by heating in substance, the decomposition of 12 and 20 stops at the stage of the monoesters 17 and 21, respectively. Competition experiments show that 1 is approximately three times less reactive towards 6c than dimethyl acetylenedicarboxylate (11). It is shown that 1 is a useful dienophile for the preparation of “mixed” [2.2]paracyclophanes of type 28.
    Notes: Acetylendicarbonsäure-di-tert-butylester (1) reagiert in guten Ausbeuten mit den Modell-Dienen 1,3-Butadien (6a), 2-Methyl-1,3-butadien (6b), 2,3-Dimethyl-1,3-butadien (6c), Furan (10) und 1,3-Cyclohexadien (19) zu den Diels-Alder-Addukten 7a-c, 12 (E = CO2C(CH3)3) und 20. Im Fall von 10 gelingt unter bestimmten Bedingungen auch die Isolierung der vier 2:1-Addukte 13 - 16 (E = CO2C(CH3)3). Während die Ester 7a - c durch Erwärmen in Gegenwart katalytischer Mengen von p-Toluolsulfonsäure bzw. beim Erhitzen in Substanz quantitativ in die entsprechenden Anhydride 8a - c übergeführt werden können, bleibt diese Zersetzung für 12 und 20 auf der Stufe der Monoester 17 bzw. 21 stehen. Wie Konkurrenzexperimente zeigen, ist 1 gegenüber 6c etwa dreimal weniger reaktiv als Acetylendicarbonsäure-dimethylester (11). Es wird gezeigt, daß 1 ein nützliches Dienophil bei der Darstellung „gemischter“ [2.2]Paracyclophane vom Typ 28 ist.
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    Die Spaltung nichtgespannter CC-Einfachbindungen in Tricarbonyleisenkomplexen 5,5-dialkylsubstituierter Cyclopentadiene (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 542-554 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cleavage of Unstrained CC Single Bonds in Tricarbonyliron Complexes of 5,5-Dialkyl-substituted CyclopentadienesCleavage of CC single bonds in η4-spirononadieneiron complex 9 is initiated by Fe2(CO)9 in boiling benzene, leading to the bridged (σ-alkyl-π-cyclopentadienyl)iron complex 10. By Fe2(CO)9 the latter is transformed to the dinuclear “propylfulvene complex” 16. The observed CC bond cleavage reactions of spirocyclopentadienes 6 can also be applied to monocyclic 5,5-dialkylcyclopentadienes 1. Crossover experiments and stereochemical results suggest an intramolecular reaction path and migration of the endo-alkyl group.
    Notes: Die Spaltung einer CC-Einfachbindung im η4-Spirononadieneisen-Komplex 9 wird durch Fe2(CO)9 in siedendem Benzol initiiert und führt zum überbrückten (σ-Alkyl-π-cyclopentadienyl)eisen-Komplex 10. Dieser reagiert - wiederum unter der Einwirkung von Fe2(CO)9 - weiter zum zweikernigen „Propylfulven-Komplex“ 16. Die an Spirocyclopentadienen 6 beobachteten Umwandlungen unter CC-Bindungsspaltung lassen sich auf offenkettige 5,5-Dialkylcyclopentadiene 1 übertragen. Aus Kreuzungsversuchen und stereochemischen Befunden kann ein intramolekularer Reaktionsverlauf unter Wanderung der endo-Alkylgruppe abgeleitet werden.
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    Einfache Synthese von 3-Acetyl-2-norbornanon durch Diels-Alder-Reaktion und Reaktivität seiner Derivate (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 555-565 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Simple Synthesis of 3-Acetyl-2-norbornanone via Diels-Alder Reaction and Reactivity of its DerivativesCyclopentadiene reacts SnCl4-catalyzed with the readily accessible benzyl ether 1b to give norbornene 2. Benzyl cleavage leads to the diol 3, on the other hand hydrogenation yields the 3-acetylnorbornanol 13 which is oxidized and methylated via 6 to 7. The acetyl group of diketone 7 reacts selectively with ylen (→ 8) and orthoformate (→ 9). With methyl lithium however the diol 12 is formed. Selective reaction of the 2-ketogroup of 2 is only possible after protecting the acetyl function in 2 (→ 5 → 14 → 10 → 19). The Grignard reaction of 2 is sterically hindered and leads with methyl or ethyl magnesium halide to 4a or b. The α,β-unsaturated ketones 16 resp. 17a and b are obtained from 4a resp. b via hydrogenation (→ 15a, b), oxidation (→ 11a, b) and dehydration.
    Notes: Cyclopentadien reagiert SnCl4-katalysiert mit dem leicht zugänglichen Benzylether 1b zum Norbornen 2. Benzylspaltung mit Natrium führt zum Diol 3, während Hydrierung das 3-Acetylnorbornanol 13 ergibt, dessen Oxidation und Methylierung über 6 zu 7 führt. Im Diketon 7 reagiert die Acetylgruppe selektiv mit Ylen (→ 8) und Orthoameisensäureester (→ 8), mit Methyllithium wird dagegen das Diol 12 gebildet. Eine selektive Reaktion der 2-Ketogruppe ist nur nach Schützen der Acetylfunktion in 2 (→ 5 → 14 → 10 → 19) möglich. Die Grignard-Reaktion von 2 ist sterisch gehindert. Sie führt mit Methyl- bzw. Ethyl-magnesiumhalogenid zu 4a bzw. b, woraus nach Hydrierung (→ 15a, b), Oxidation → 11a, b), und Wasserabspaltung die α,β-ungesättigten Ketone 16 bzw. 17a und b erhalten werden.
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    Addition von Aldehyden an aktivierte Doppelbindungen, XXII. Addition von aliphatischen Aldehyden an α,β-ungesättigte Carbonsäureester und Nitrile (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 690-698 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Addition of Aldehydes to Activated Double Bonds, XXII. Addition of Aliphatic Aldehydes to α,β-Unsaturated Esters and NitrilesThiazolium salt catalysed addition of aliphatic aldehydes to α,β-unsaturated esters and nitriles leads to γ-ketocarboxylic esters (1 - 24) and γ-ketonitriles (25 - 32).
    Notes: Aliphatische Aldehyde addieren thiazoliumsalz-katalysiert an α,β-ungesättigte Carbonsäureester und Nitrile unter Bildung von γ-Ketocarbonsäureestern (1 - 24) und γ-Ketosäurenitrilen (25 - 32).
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    Urofuransäuren - eine bisher unbekannte Klasse von Stoffwechselprodukten (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 699-709 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Urofuranic Acids - a Hitherto Unknown Class of Metabolic CompoundsBy a combination of chromatographic methods 1 mg of pentylurofuranic acid, a dicarboxylic acid C14H20O5, was isolated from 10 1 urine. According to spectroscopic measurements in combination with reactions in microscale its structure is 3-carboxy-4-methyl-5-pentyl-2-furanpropanoic acid (1a). This was confirmed by synthesis. Pentylurofuranic acid does not only occur in urine, but also in blood. Accompanying compounds differ only in the construction of the side chain in position 5.
    Notes: Aus 10 1 Harn wurde durch Kombination verschiedener chromatographischer Verfahren 1 mg Pentylurofuransäure, eine Dicarbonsäure C14H20O5, isoliert. Ihr kommt nach spektroskopischer Untersuchung in Kombination mit Mikroabbaureaktionen die Konstitution 3-Carboxy-4-methyl-5-pentyl-2-furanpropansäure (1a) zu, die durch Synthese gesichert wurde. Die Pentylurofuransäure kommt nicht nur im Harn (0.5-2 mg/24 h), sondern auch im Blut vor. Begleitverbindungen unterscheiden sich von ihr nur durch den Bau der Seitenkette in Stellung 5.
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    Asymmetrische Synthesen, V. Optisch aktive 5-Amino-4-phenyl-1,3-dioxane und deren Einfluß auf die Stereoselektivität der asymmetrischen Strecker-Synthese (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 710-721 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Asymmetric Syntheses, V. Optically Active 5-Amino-4-phenyl-1,3-dioxanes and Their Influence on the Stereoselectivity of the Asymmetric Strecker-SynthesisFrom (1S, 2S)-(+)-2-amino-1-phenyl-1,3-propanediol (1) and aldehydes or ketones 2a - e, respectively, the appropriate 5-amino-4-phenyl-1,3-dioxanes 3a - e are prepared. With benzaldehyde they form well crystallizing azomethines 4a - e. The conformation and configuration of 3a - e and 4a - e are deduced spectroscopically. From these results, and from investigations of the epimer equilibria 5a - e/6a - e conclusions are drawn about the stereochemical course of the asymmetric Strecker-synthesis.
    Notes: Aus dem (1S, 2S)-(+)-2-Amino-1-phenyl-1,3-propandiol (1) werden mit den Aldehyden bzw. Ketonen 2a - e die entsprechenden 5-Amino-4-phenyl-1,3-dioxane 3a - e hergestellt, die mit Benzaldehyd die gut kristallisierenden Azomethine 4a - e bilden. Die Konformation und Konfiguration von 3a - e und 4a - e werden spektroskopisch bestimmt. Aus diesen Ergebnissen und den Untersuchungen über das Epimerengleichgewicht 5a - e/6a - e lassen sich Rückschlüsse auf den stereochemischen Verlauf der asymmetrischen Strecker-Synthese ziehen.
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    Beiträge zur Chemie des Bors, CV. (N-Lithiomethylamino)dimethylboran als Reagens zur Darstellung N-funktioneller Aminodimethylborane (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 728-738 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Boron, CV. (N-Lithiomethylamino)dimethylborane as a Reagent for the Preparation of N-Functional AminodimethylboranesThe reagent (CH3)2 — N(CH3)Li (1) allows the synthesis of many borylaminoelement compounds such as (CH3)2B — NCH3 — BCH3 — N(CH3)2, (CH3)2Si[NCH3 — B(CH3)2]2, (CH3)2B - NCH3 — Si(CH3)2 — NCH3 — Si(CH3)2Br, (CH3)2B — NCH3 — P(CH3)2 or (CH3)2B — NCH3 — As(CH3)2. Multifunctional element halides cause the formation of a complex mixture of products, and this is in part due to cyclocondensation reactions of longer chain compounds.
    Notes: Das Reagens (CH3)2B — N(CH3)Li (1) ermöglicht die Synthese zahlreicher Borylaminoelement-Verbindungen wie (CH3)2B — NCH3 — BCH3 — N(CH3)2, (CH3)2Si[NCH3 — B(CH3)2]2, (CH3)2B — NCH3 — Si(CH3)2 — NCH3 — Si(CH3)2Br, (CH3)2B — NCH3 — P(CH3)2 oder (CH3)2B — NCH3 — As(CH3)2. Mit mehrfunktionellen Elementhalogeniden wird die Produktpalette komplexer, was auch auf Cyclokondensation der längerkettigen Verbindungen zurückzuführen ist.
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    Neue Kondensationsreaktionen an 4-Hydroxy-3-oxo-2,5-diphenyl-2,3-dihydrothiophen-1,1-dioxid (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 750-756 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Condensation Reactions of 4-Hydroxy-3-oxo-2,5-diphenyl-2,3-dihydrothiophene 1,1-Dioxide4-Hydroxy-3-oxo-2,5-diphenyl-2,3-dihydrothiophene 1,1-dioxide (1) reacts with primary amines according to their basicity to give the compounds 6a - h, and 7, resp.; with hydrazines the monohydrazones (8a - d) are obtained. Condensation with aliphatic diamines leads only in the case of 1,1-ethanediamine to a ring system (2), with the higher homologues to bridged compounds (3a - c). Reaction with methylenediamine dihydrochloride leads to the same product (5) as with ammonia. Active derivatives of carboxylic acids react with 1 to give mono- (9a,b) or bisacylation (10), in the case of thiophosgene the corresponding dioxole 11 is formed. With trialkyl phosphites 1 produces the vinylogue sulfonic esters 12a, b by simple alkylation, analogous to the reaction with diazomethane.
    Notes: 4-Hydroxy-3-oxo-2,5-diphenyl-2,3-dihydrothiophen-1,1-dioxid (1) reagiert mit primären Aminen je nach deren Basizität zu den Verbindungen 6a - h oder 7; mit Hydrazinen erfolgt Monohydrazonbildung zu 8a - d. Kondensation mit aliphatischen Diaminen führt nur im Falle des 1,2-Ethandiamins zum ringgeschlossenen Produkt (2), höhere homologe Diamine bilden verbrückte Verbindungen (3a - c). Die Reaktion mit Methandiamin-dihydrochlorid führt zu Produkt 5, das auch durch Umsetzung mit Ammoniak erhalten wird. Aktive Carbonsäurederivate setzen sich mit 1 zum Mono- (9a, b) bzw. Bisacylprodukt (10) um. Mit Thiophosgen liefert 1 das Dioxol 11; mit Trialkylphosphiten erfolgt Alkylierung zu den vinylogen Sulfonsäureestern 12a, b analog der Umsetzung mit Diazomethan.
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    Bis(pentamethylcyclopentadienyl)germanium und -zinn sowie (Pentamethylcyclopentadienyl)germanium- und -zinn-Kationen: Synthese, Struktur und Bindungsverhältnisse (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 757-769 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(pentamethylcyclopentadienyl)germanium and -tin and (Pentamethylcyclopentadienyl)germanium- and -tin Cations: Synthesis, Structure, and Bonding PropertiesSynthesis and properties of bis(pentamethylcyclopentadienyl)germanium (2) and -tin (1) and of the ionic (pentamethylcyclopentadienyl)germanium- and -tin tetrafluoroborates 4 and 3 are described. The structures of 1 - 4 result from spectroscopic and analytical data and in the case of 1 and 3 also from X-ray structure analyses. The bonding in 1 - 4 is discussed on the basis of model MO calculations.
    Notes: Synthese und Eigenschaften des Bis(pentamethylcyclopentadienyl)germaniums (2) und -zinns (1) sowie der ionischen (Pentamethylcyclopentadienyl)germanium- und -zinn-tetrafluoroborate 4 und 3 werden beschrieben. Die Strukturen von 1 - 4 resultieren aus spektroskopischen und analytischen Daten sowie im Falle von 1 und 3 auch aus Röntgenstrukturanalysen. Elektronenstruktur und Bindungsverhältnisse in 1 - 4 werden auf der Basis von MO-Modellrechnungen diskutiert.
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    Thermolyse von Oxazolin-5-onen, X. 3-Imidazoline und Δ3-Tetrahydropyrimidine durch Thermolyse von 3-Oxazolin-5-onen aus N-Acyldipeptiden (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 770-786 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermolysis of Oxazolin-5-ones, X. 3-Imidazolines and Δ3-Tetrahydropyrimidines by Thermolysis of 3-Oxazolin-5-ones Derived from N-Acyl DipeptidesOn thermolysis 2-(acylaminomethyl)-3-oxazolin-5-ones (3a - g) undergo elimination of CO2 to give nitrile ylides which cyclize to 3-imidazolines 4a - g via intramolecular proton transfer. The 2-acylaminoethyl derivative 3h yields a Δ3-tetrahydropyrimidine 5h in an analogous manner. Compounds 3 may be easily obtained from N-acyl dipeptides 1. The temperature dependence of the 1H NMR spectra of 4 is discussed.
    Notes: Die Thermolyse von 2-(Acylaminomethyl)-3-oxazolin-5-onen (3a - g) führt unter Eliminierung von CO2 zu Nitril-yliden, welche nach innermolekularer Protonenübertragung zu 3-Imidazolinen 4a - g cyclisieren. Analog liefert das 2-(Acylaminoethyl)-Derivat 3h ein Δ3-Tetrahydropyrimidin 5h. Die Oxazolinone 3 sind aus N-Acyldipeptiden 1 leicht zugänglich. Die Temperaturabhängigkeit der 1H-NMR-Spektren von 4 wird diskutiert.
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    Stereoselektive Synthesen von Alkoholen, IV. Konformationseinflüsse auf die Stereochemie der Allylsulfoxid-Sulfensäure-allylester-Umlagerung (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 856-863 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Stereoselective Synthesis of Alcohols, IV. Conformational Factors Determining the Stereochemistry of the Allyl Sulfoxide/Allyl Sulfenate-RearrangementThe stereochemistry of the [2,3]sigmatropic rearrangement of the conformationally rigid allyl sulfoxides 5 revealed a 6.2 fold preference for axial formation of the new C — O-bond. This preference dominates the 3.1 fold preference for an exo-versus endo-transition state. These data form the basis for a discussion of the stereochemistry of rearrangement of the conformationally flexible allyl sulfoxides 1 and 13.
    Notes: Aus der Stereochemie der [2,3]sigmatropen Umlagerung der konformativ fixierten Allylsulfoxide 5 kann man eine 6.2-fache Präferenz für eine axiale Neuknüpfung der C — O-Bindung ableiten, die über eine 3.1-fache Präferenz für einen exo-Übergangszustand dominiert. Diese Vorstellungen wurden auf die Umlagerung der konformativ flexiblen Allylsulfoxide 1 und 13 übertragen.
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    Kumulierte Ylide, VII. Eine Methode zum Aufbau α,β-ungesättigter Carbonsäurederivate (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 912-918 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cumulated Ylides, VII. A Method for the Synthesis of α,β-Unsaturated Carboxylic CompoundsPhosphacumulene ylides 1 add alcohols, thiols, and NH-acidic compounds to form phosphoranes 3, which react with aldehydes to give esters, thiol esters, imidates, thioimidates, amidines, azolides, and sulfonamides of α,β-unsaturated carboxylic acids.
    Notes: Phosphacumulen-Ylide 1 addieren Alkohole, Thiole und NH-acide Verbindungen zu Phosphoranen 3, die sich mit Aldehyden zu Estern, Thiolestern, Imidsäureestern, Imidsäurethioestern, Amidinen, Azoliden sowie Sulfonamiden α,β-ungesättigter Carbonsäuren umsetzen lassen.
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    Derivatives of Aza-nido-tetraborane and Diaza-arachno-pentaborane from Tri-tert-butylazadiboriridine (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1-9 
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    ISSN: 0009-2940
    Keywords: 1-Aza-nido-tetraboranes ; 2,5-Diaza-arachno-pentaboranes ; 2,5-Diaza-nido-hexaboranes ; Boryl[diborane(4)yl]amine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Lewis acids RBH2 are added to the basis B-B bond of tri-tert-butylazadiboriridine, NB2tBu3 (1a), to give 5-alkyl-1,2,3-tri-tert-butyl-1-aza-nido-tetraboranes of type 3 (two endo-H atoms at B5) or type 4 (one H atom in a B2-B5 bridging position, one exo-H atom at B5), either as a mixture of 3 and 4 (3, 4b-d: R = Me, tBu, CMe2iPr) or with the isomer 4 in high excess (4e, f: R = Ph, sBu). The reaction of dialkylboranes R2BH with 1a yields 5,5-dialkyl-1,2,3-tri-tert-butyl-1-aza-nido-tetraboranes of type 4 (one H atom in a B2-B5 bridging position; 4g, h: R2 = Et2, cycloocta-1,5-diyl). In boiling THF, trialkylboranes BR3 transform 1a into NB2tBu2R which, expectedly, dimerizes spontaneously to give a dialkyltetra-tert-butyl-2,5-diaza-nido-hexaborane of type 2 (2a, b: R = Me, Et). The products of the addition of aminoboranes H2B=NRR' to 1a are identified as alkyl derivatives of 2,5-diaza-arachno-pentaborane, N2B3tH2tBu3RR' (5a-d, R/R' = H/Pr, H/tBu, Me/Me, Et/Et). The aminoborane H2B = NiPr2 with a sterically more demanding amino group hydroborates the B-B bond of 1a to give the acyclic product iPr2N=BH-B(tBu)-N(tBu)=B(tBu)H (6). In contrast to the B atoms, the N atoms in the electron-deficient cluster skeletons of 2-5 need not take part in (3c,2e) bonds of the s̰ type. The molecular structures of 4c, 5d, and 6 are confirmed by X-ray structural analyses.
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    New Pathways in Tellurium-Chalkogen-Nitrogen Chemistry: Preparations, Structures, and Properties of Telluraheterocycles (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 11-22 
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    ISSN: 0009-2940
    Keywords: Thiaselenatelluradiazoles ; Thiaselenatelluratetrazocinium ; Tellurium(IV) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of Se(NSO)2 with TeF4 in CH2Cl2 yields the compounds (4a) and (5b), while with TeBr4 after six months (2d) is formed. An almost quantitative yield of Cl4Te2N4S2 (6) is obtained from either Cl6Te2N2S (1a) and (CH3)3SiNSNSi(CH3)3 in CH2Cl2 at 20°C (2 d) or TeCl4 and (CH3)3SiNSO (molar ratio 1:2) in CH2Cl2 at 60°C (3 d). The use of (CH3)3SiOSi(CH3)3 as solvent in the last mentioned procedure gives 1a and small amounts of Cl2Te(NSO)2. Similarly, F2Te(NSO)2 is prepared from TeF4 and (CH3)3SiNSO in CH2Cl2. Dechlorination of 1a with (C6H5)3Sb leads to (2a), which is also produced from TeCl4 and [(CH3)3Si]2NSN[Si(CH3)3]2. When TeF4 is used instead of TeCl4 (molar ratio 3:1) the salt (7a) is formed. Similarly, (7b) is prepared from 2a and AsF5 or Ag+[AsF-6] in SO2. A new method for the preparation of bicyclic type 1 telluraheterocycles involves bromination of 2a yielding Cl2Br4Te2N2S (1b). Dehalogenation with (C6H5)3Sb converts 1b into (2b). When 2b is treated with Br2 in CH2Cl2 an oxidative halogenation takes place with formation of Br6Te2N2S (1c). Metathetical exchange between 2b and Ag+[AsF-6] gives (7c). Isostructural S(NSO)2 reacts with TeCl4 for several weeks at 60°C in CH2Cl2 to form S4N4. TeCl4 and [S5N+5][Te3Cl-3], in contrast to the corresponding reaction with Se(NSO)2. The molecular structures of 4a, 7b, 8, and [S5N+5][Te3Cl-13] have been determined by X-ray diffraction methods. Spectroscopic data for all new compounds are presented.
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    Tellurium Polycations by Oxidation of Tellurium with Tungsten Halides Syntheses and Crystal Structures of Te6(WOCl4)2 and Te6I2(WCl6)2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 23-27 
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    ISSN: 0009-2940
    Keywords: cyclo-Hexatellurium(2+) ; 1,4-Diiodo-cyclo-hexatellurium(2+) ; Hexachlorotungstate(V) ; Tetrachlorooxotungstate(V) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: WOCl4 reacts at 200°C with tellurium in a sealed, evacuated ampoule with the formation of Te6(WOCl4)2. The structure consists of six-membered tellurium rings in a boat conformation with significant transannular interactions and of pyramidal WOCl4 units which are linked by linear asymmetric O...;W=O bridges to polymeric (WOCl4)n, chains. The observed paramagnetism is consistent with the ionic formulation Te2+6[(WOCl-4)2]n. In the reaction of WCl6, I2 and Te in a 2:1:6 ratio Te6I2(WCl6)2 is formed at 150°C. The crystal structure consists of Te6I2+2cations and of slightly distorted octahedral WCl-6 anions. The Te6I2+2 ions are isostructural with Se6I2+2 and consist of a six-membered ring of Te atoms in the chair conformation with two I atoms bound in the 1,4-positions.
    Additional Material: 6 Ill.
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    Two Alternatives of Heteroallene Insertion in Metal  -  Ligand Bonds of Five-Coordinate Ruthenium(II) and Osmium(II) Complexes [MXY(CO)(PiPr3)2]Herrn Professor Nils Wiberg zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 41-47 
    Details
    ISSN: 0009-2940
    Keywords: Ruthenium complexes ; Osmium complexes ; Insertion reactions ; Carbon disulfide ; Carbon dioxide ; Methyl isothiocyanate ; Zwitterionic ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The five-coordinate chloro(hydrido)- and hydrido(iodo)ruthenium(II) and -osmium(II) compounds [MHX(CO)(PiPr3)2] (1, 2, 6, 7) react with CS2 to give the octahedral dithioformato complexes [MCl(CO)(PiPr3)2(η2-S2CH)] (3, 4, 8, 9) in excellent yields. In the initial step, an addition of the heteroallene to the metal center occurs which is followed by insertion of CS2 into the M - H bond. On treatment of the dichlororuthenium(II) derivative [RuCl2(CO)(PiPr3)2] (10), which is prepared from RuCl3 · aq and PiPr3 in methanol, with carbon disulfide insertion into one of the Ru - PiPr3 bonds takes place to give the six-coordinate ruthenium(II) complex 12 with zwitterion -S2CPiPr3+ as a chelating ligand. While the reaction of [OsH(SPh)(CO)(PiPr3)2] (13) with MeSCN leads to addition of the thionitrile to the metal center, the starting material reacts with MeNCS by insertion of the heteroallene into the Os - SPh bond to give two stereoisomers 15a, b, in which the nitrogen atom of the chelate ring is either cis or trans to the hydrido ligand. The octahedral methoxydithiocarbonato- and formatoosmium(II) compounds 16 and 17 are prepared from 2 and CS2 or CO2 in the presence of NaOMe. The crystal and molecular structures of 4 (M = Os), 12 and 15a have been determined.
    Additional Material: 3 Ill.
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    Synthese und Struktur von Cobalt(III)-Komplexen mit doppelt deprotoniertem Anhydroerythrit, Methyα-D-mannopyranosid und Methyl-β-D-galactopyranosid (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 75-79 
    Details
    ISSN: 0009-2940
    Keywords: Cobalt(III) complexes ; Dianionic polyolato ligands ; Anhydroerythritol ; α-DMannopyranoside, methyl ; α-DGalactopyranoside, methyl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyol Metal Complexes, XII[1].  -  Synthesis and Structure of Cobalt(III) Complexes with Doubly Deprotonated Anhydroerythritol, Methyl α-DMannopyranoside, and Methyl α-DGalactopyranosideThe polyols anhydroerythritol (AnEryt), methyl α-D-mannopyranoside (Me-α-D-Manp), and methyl α-D-galactopyrano-side (Me-α-DGalp) are deprotonated twice to form the cobalt(III) complexes [(en)2Co(AnErytH-2)]I (1), δ-[(en)2- Co(Me-α-DManp3,4H-2)]ClO4 · NaClO4 · 2H2O (2), and δ-[(en)2Co(Me-α-DGalp2,3H-2)]ClO4·H2O (3), resp., in aqueous, alkaline solutions of trans-[(en)2CoCl2]Cl. The crystal structures of 1-3 have been determined by X-ray diffraction.
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    URL: http://dx.doi.org/10.1002/cber.19951280111
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    Contribution to the Chemistry of Boron, 222.  -  Chemistry of Diborane(4) Derivatives: Mixed Tetraaminodiboranes(4) and Additions of Diborane(4) Derivatives to an Amino-imino-borane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 93-93 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280115
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    Protolysis of Tri-tert-butylazadiboriridine: Formation of a B-H-B Bridge in Unusual Coordination (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 99-103 
    Details
    ISSN: 0009-2940
    Keywords: Tri-tert-butylazadiboriridine ; (Hydroboryl)(methoxyboryl)amine ; 2,3-μ-Hydro-1,2,3-azoniadiborata-l-cyclopropenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The B—B bond of tri-tert-butylazadiboriridine [—NR—BR—BR—] (R = tBu; 1) is oxidized by MeOH to give the (hydroboryl)(methoxyboryl)amine H—BR=NR-BR(OMe) (2a). μ-2,3-Hydroazoniadiborata-1-cyclopropenes [=NR—BR(X)—μH—BR=] (3a, 3c-e) are formed by the action of the acids HX upon 1. A similar hydrogen bridge as in 3a-e is formed during the hydroboration of 1 by catecholborane, yielding 3f. A B atom is identified in the products 3a-f to be planarly coordinated by four atoms, two of which are forming a BHB three-center bond with that B atom. This is a novel bonding situation in boron chemistry. The structures of the products are deduced from 1H-, 11B-, and 13C-NMR spectra and are confirmed by X-ray structural analyses of 2a, 3a, and 3c.
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    Synthese und Struktur zweikerniger Kupfer(II)-Komplexe eines neuen Hexaaza-Makrocyclus mit verbrückenden Oxalat- und Acetat-Ionen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 115-119 
    Details
    ISSN: 0009-2940
    Keywords: Polyazamacrocycles ; Dinucleating ligands ; Copper complexes ; Oxalate complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of Dinuclear Copper(II) Complexes of a Novel Hexaaza Macrocycle Containing Bridging Oxalate and Acetate IonsNon-template Schiff base [2 + 2] condensation of pyridine-2,6-dicarbaldehyde with 1,4-diamino-2-butyne yields the hexaazamacrocyclic ligand 1, which is converted to 2 by NaBH4 reduction of the imino groups. Two dinuclear copper(II) complexes of 2 containing oxalate and acetate ions, [(2)Cu2(μ-C2O4)](BPh4)2 (3) and [(2)Cu2(μ-CH3CO2)(OH2)](PF6)2.25-(NO3)0.75 (4), were characterized by X-ray crystallography. The oxalate ligand in 3 forms a (μ-η4:η4) bridge between the copper atoms. Compound 4 contains a syn-anti-bridging acetate ion. The Cu-Cu distances are 5.315 Å in 3 and 4.746 Å in 4, respectively. Oxalate can be separated from other carboxylates in aqueous solution by selective binding to the [(2)Cu2] unit and precipitation of 3.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280205
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    Synthesis, X-Ray Crystal Structure and Magnetic Characterization of the First “Ni3S4N3” Nickel Thiolate Cluster (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 125-129 
    Details
    ISSN: 0009-2940
    Keywords: Nickel cluster ; Nickel thiolate ; Hydrogenase ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tridentate N,O,S-ligand (RS)-2-[(2-mercapto-1-methylamino)ethyl]phenol (rac-1) was prepared from ortho-hydroxy-chloroacetophenone in three steps. When this ligand was treated with nickel(II) acetate, the novel “Ni3S4N3” cluster rac-3 was obtained. The X-ray crystal structure of rac-3 unambiguously revealed the pseudo-C3 symmetric structure of this novel nickel cluster, which is made up by three nickel ions, one sulfide sulfur atom, and three homochiral ligand molecules, each contributing one thiolate sulfur atom and one amine nitrogen atom to the ligation of the metal ions. According to NMR-spectroscopic results, this highly symmetric structure is maintained in solution. The magnetic studies revealed diamagnetic behavior in the solid state, although antiferromagnetic interaction of the metal centers cannot absolutely be excluded.
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    URL: http://dx.doi.org/10.1002/cber.19951280207
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    Stereospecific Ligand Substitutions in Manganese(I) Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 151-155 
    Details
    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Phosphane ligands ; Thioethers ; Manganese complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of fac-[(P2SPh-P,P')Mn(CO)3Br] and fac-[(PS2Ph-P,S)Mn(CO)3Br] [P2SPh: Z = PPh2; PS2Ph: Z = SPh in CH3C-(CH2PPh2)(CH2SPh)(CH2Z)] with silver hexafluorophosphate yields the η3-tripodal manganese complexes [(P2SPh-P,P',S)Mn(CO)3]PF6 (7) and [(PS2Ph-P,S,S')Mn(CO)3]PF6 (9), respectively, whereas the reaction of CH3C(CH2PPh2)2-(CH2SH) with Mn(CO)5Br gives directly [CH3C(Ph2-PCH2)2(CH2S)-P,P',S]Mn(CO)3 (11). Both ionic complexes 7 and 9 undergo stereospecifically ligand substitution upon treatment with Br-, I-, N-3, SCN- and CN- to give syn-fac-[(P2SPh-P,P')Mn(CO)3X] and syn-fac-[(PS2Ph-P,S)Mn(CO)3X] (X = Br, I, SCN, N3, CN) respectively, but the neutral complex 11 fails to undergo such a substitution reaction with these ions. However, reaction of I- with the complex [(PSMe)-P,P',S]Mn(CO)3]BF4 (20) [P2SMe = CH3C(CH2-PPh2)2(CH2SCH3)), which is obtained from the S-alkylation of 11 with (CH3)3OBF4, affords syn-fac-[(P2SMe)-P,P']Mn(CO)3I (22s) exclusively. The possible reaction mechanism of this ligand substitution is discussed.
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    Oxacycloalkenyliden-Komplexe von Chrom, Molybdän und Wolfram: Synthese, Anellierung mit Alkinen und Diels-Alder-Reaktionen mit Dienen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 157-161 
    Details
    ISSN: 0009-2940
    Keywords: Carbene ligands ; Chromium complexes ; Molybdenum complexes ; Tungsten complexes ; Annulation reaction ; Diels-Alder reaction ; Oxacyclopentenylidene ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of Complex Ligands, LXI[1]. - Oxacycloalkenylidene Complexes of Chromium, Molybdenum, and Tungsten: Synthesis, Their Annulation with Alkynes and Diels-Alder Reaction with DienesLithiiated propargylic ether 1 reacts with M(CO)6 (M = Cr, Mo, W) to give the 2-oxacyclic carbene complexes 2-4 containing an α,β-double bond and a cyclic acetal structure which serves as a protected benzoyl group. Reaction of the chromium complex 2 with tolan leads to an acyl hydroquinone derivative 5. The tungsten complex 3 undergoes a [4 + 2] cycloaddition with cyclopentadiene to give two diastereomeric oxatricyclic carbene complexes 6 and 7 with an endo/exo selectivity of 3:1. The stereochemistry of the Diels-Alder reaction is controlled by the configuration of the acetal carbon center.
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    URL: http://dx.doi.org/10.1002/cber.19951280212
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    Darstellung und Komplexierung von 1,4-Dimethyl-2,3-bis(isopropyliden)-1,4-diboratetralinHerrn Professor Nils Wiberg zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 183-185 
    Details
    ISSN: 0009-2940
    Keywords: 1,4-Diboranaphthalines ; 2,7-Diboradodeca-1,3,9,11-tetraenes ; Cobalt complexes ; Rhodium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Complexation of 1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline (2) is obtained from o-dilithiumbenzene and 2,5-dimethyl-3,4-bis(chloromethylboryl)-2,4-hexadiene in 61% yield. Its complexation with cyclopentadienylbis(ethene)cobalt leads to the triple-decker bis(η5-cyclopentadienylcobalt)-μ-η6,η6-1,4-dimethyl-2-isopropenyl-3-isopropyl-1,4-dihydro-1,4-dibora-naphthaline (3) in low yield. However, the reaction of 2 with (C5H5)Rh(C2H4)2 and (C5Me5)Co(C2H4)2 originates complexes of a tricyclic ligand formed from 2 via conrotatoric [2 + 2] cycloaddition of the isopropylidene groups. (η5-Cyclo-pentadienylrhodium)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (4), (η5-pentamethylcyclopentadienylcobalt)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (5) and its related dinuclear complex 6 could be isolated in 29, 10, and 31%, respectively. Their constitutions are derived from spectroscopic data and proven by X-ray structure analysis of 4.
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    Zerfall von Nitrosylazid, N4O: Existieren auch cyclische Stickstoff-Oxide? (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 201-203 
    Details
    ISSN: 0009-2940
    Keywords: Nitrogen oxides ; Calculations, ab initio ; Tetranitrogen monoxide ; Dinitrogen monoxide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Decomposition of Nitrosyl Azide, N4O: Are Cyclic Nitrogen Oxides Existent?The unimolecular decomposition of nitrosyl azide (tetranitrogen monoxide), N4O, was studied at the electron-correlated, spin-restricted RMP2 level with the 6-31G(d,p) and 6-31+G* basis sets. Frequency calculations were performed at 6-31+G* on the optimized structures. It is demonstrated that the experimentally established trans-trans-N4O (Cs) may either interconvert into cis-cis-N4O which upon decomposition forms cyclic N4O (C2v) as an intermediate species to finally give N2O (C∞v) and N2, or trans-trans-N4O may directly dissociate into cyclic N2O (C2v) and N2. All structures determined were rationalized by energy hypersurface calculations.
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    Reactions of Diazo Compounds and Chiral Rhenium Alkylidene Complexes of the Formula [(η5-C5H5)Re(NO)(PPh3)(=CHR)]+ PF-6 A Versatile and Highly Stereoselective Route to Alkene Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 213-220 
    Details
    ISSN: 0009-2940
    Keywords: Rhenium complexes ; Alkylidene complexes ; Diazo compounds ; Alkene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The methylidene complex [(η5-C5H5)Re(NO)(PPh3)(=CH2)]+ PF-6 or the Re—CD2 analog react with diazo compounds N2CHR [R — H, Si(CH3)3, COPh, CO2C2H5] in CH2Cl2 at -80°C to give alkene complexes [(η5-C5H5)Re(NO)(PPh3)(η2-H2C=CHR)]+ PF-6 or D2C=CHR analogs. The two Re=C geometric isomers of benzylidene complex [(η5-C5H5)Re-(NO)(PPh3)(=CHPh)]+ PF-6 and CH2N2 react to give opposite configurational diastereomers of styrene complex [(η5-C5H5)Re(NO)(PPh3)(η2-H2C=CHPh)]+ PF-6. Stereochemical features of these reactions are analyzed in detail, and are interpreted in terms of models involving (a) attack of the diazo compound upon the Re=C face opposite to the bulky PPh3 ligand, (b) an antiperiplanar disposition of the Re=C and C—N2 bonds in the transition state, utilizing the diazo carbon face that minimizes interactions of the substitutent (R) and cyclopentadienyl ligand, and (c) N2 loss from the resulting intermediate [(η5-C5H5)Re(NO)(PPh3)(CHR′CHRN2)]+ PF-6 via a conformer with antiperiplanar P—Re—CHR′—C and Re—CHR′—CHR—N linkages, with anchimeric assistance of the rhenium fragment d orbital HOMO from the backside.
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    Contributions to the Chemistry of Boron, 227Part 226: Ref.. The P-centered Chemistry of [(Di-tert-butylphosphanyl)imino]-(2,2,6,6-tetramethylpiperidino)boraneDedicated to Professor Helmut Werner on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 205-212 
    Details
    ISSN: 0009-2940
    Keywords: Borane, [(di-tert-butylphosphanyl)imino](2,2,6,6-tetramethylpiperidino) dimer ; Phosphonium, di-tert-butylmethyl[(2,2,6,6-tetramethylpiperidinoborylene)imino]iodide ; Haloboration ; Hydroboration ; Metal carbonyl complexes of [(di-tert-butylphosphanyl)imino](2,2,6,6-tetramethylpiperidino)borane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The elements oxygen, sulfur, and selenium add to the P atom of the title borane 1. In contrast to the formation of tmp—B≡N—P(X)tBu2 (X = S, Se), the P oxide (X = O) dimerizes to [tmp—B≡N—P(O)tBu2]2 (5) with an eight-membered flat boat-shaped B2N2P2O2 ring. Borane 1 reacts readily with Mel to yield a phosphonium salt 8 and with BBr3 to give an adduct 9 with a B—P bond. In contrast, bis(dichloroboryl)-methane not only adds to 1 to generate a coordinate B—P bond but also chloroborates the B≡N triple bond, the final product being a new five-membered heterocycle 10. Similarly, the BH3 component of BH3·SMe2 first adds to the P atom of 1 followed by reaction of a second mol of BH3·SMe2 which hydroborates the B≡N triple bond. Finally, metal carbonyl fragments add only to the P atom of 1, demonstrating also that the chemistry of the molecule 1 is dominated by the basicity of its P center.
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    Synthese und Charakterisierung stabiler Bis(phosphonio)isophosphindolylium-Carbonylmetallate und eines kationischen Bis(phosphonio)isophosphindolylium-Gold-KomplexesHerrn Professor Alfred Schmidpeter zum 65. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 259-266 
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    ISSN: 0009-2940
    Keywords: Bis(phosphonio)isophosphindolylium cation ; Gold complexes ; Bis(phosphonio)isophosphindolylium carbonylmetallates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Characterisation of Stable Bis(phosphonio)isophosphindolyliumcarbonylmetallates and a Cationic Bis(phosphonio)isophosphindolylium-Gold ComplexHerrn Professor Alfred Schmidpeter zum 65. Geburtstag gewidmet.Reaction of 1,3-bis(triphenylphosphonio)isophosphindolylium bromide, [L+][Br-] (1a), with Tl[Co(CO)4], Na[MoCp-(CO)3], or Na[WCp(CO)3] (5a-c) yields the corresponding ionic isophosphindolylium-carbonylmetallates, 6a-c. Whereas 1a fails to react with neutral metal carbonyls, a mixture of ionic complexes of the type [LAuX+][AuYZ-] (7a, X, Y, Z = Cl or Br) is formed by reaction with two equivalents of AuCl. Treatment of AuCl with the triflate [L+][OTf-] (1b), which is accessible from 1a via anion metathesis, furnishes [LAuCl+][OTf-] (7b). Both the carbonylmetallate 6c and the complex 7b have been characterized by X-ray structure analyses. 7b displays enhanced reactivity as compared to 1b towards MeOH and H2O, forming the addition products 8 and 9a, b, the latter existing as two different diastereomers. Reactions of 7b with LiF, (Me2N)3P=O, and (Et2N)2C=NH), respectively, proceed via ligand exchange to yield equilibrium mixtures containing the cations [L+] and [LAuCl+].
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    Darstellung von phosphor- und fluorhaltigen Calix[4]aren-Derivaten. Konformationsanalyse, Trennung der Konformere und Röntgenstrukturanalyse an einem KonuskonformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 267-273 
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    ISSN: 0009-2940
    Keywords: Calix[4]arenes ; Supramolecular chemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of Phosphorus -  and Fluorine-Containing Calix[4]arene Derivatives. Conformational Analysis, Separation of the Conformers, and X-Ray Crystal Structure Analysis of a Cone ConformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet.The Calix[4]arene 1 reacts with hexamethyldisilazane or (diethylamino)trimethylsilane to form the bis-trimethylsilyl-ated derivative 2. Treatment of 2 with PF2C1 gives the mono-and bis-difluorophosphites 3 and 4, which react with elimination of Me3SiF or PF3 to yield the monofluorophosphite derivative 5. All four OH hydrogen atoms in 1 are replaced by lithium on reaction with nBuLi with formation of the tetrali-thiated product 6. This has been allowed to react with the Pchlorophosphorinanones 7-9. From 7 the cone conformer 10a is formed, whereas in the case of 8 and 9 a mixture of all four possible conformars 11a-d and 12a-d is obtained. The pure conformers 12a-d are isolated. By refluxing the cone conformer 12a in tetrachloroethane a conformational conversion is effected. In order to evaluate its coordinating ability, 12a was allowed to react with dichloro(cycloocta-1, 5-diene)platinum(II) to form the trans-disubstituted complex 13. In the case of 12a (acetonitrile solvate) a single-crystal X-ray structure analysis has been conducted. The molecule displays a cone conformation, whereby two of the opposing phenyl rings are approximately parallel and the other two approximately perpendicular to each other.
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    URL: http://dx.doi.org/10.1002/cber.19951280310
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    Electronic Resource
    Synthese kationischer η2-Phosphinocarben-Komplexe des Molybdäns und WolframsHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 289-292 
    Details
    ISSN: 0009-2940
    Keywords: η2-Phosphinocarbene complexes of molybdenum and tungsten ; Carbyne complexes ; Chlordimethylphosphane ; Chlordiphenylphosphane ; Electrophilic addition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of Cationic η2-Phosphinocarbene Complexes of Molybdenum and TungstenHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet.The reaction of chlordimethylphosphane or chlordiphenyl-phosphane and sodium tetraphenylborate with dicarbonyl(η5-cyclopentadienyl)carbyne complexes of molybdenum and tungsten enables the direct conversion of a M=CR group into a M=C(R)—PR2 unit providing dicarbonyl substituted η2-phosphinocarbene complexes in high yields. In the absence of Na[BPh4] a base induced carbonyl carbene coupling reaction affords η3-phosphinoketene complexes.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280313
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