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  • 1
    Electronic Resource
    Electronic Resource
    Die Umsetzung des Trimethylphosphats mit Hexamethylphosphorsäuretriamid - eine rationelle Synthese eines CyclotriphosphatsProfessor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 177-180 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Trimethylphosphate with Hexamethyl Phosphoric Acid Triamide - a Versatile Synthesis of a CyclotriphosphateThe reaction of the two title compounds 5 and 6 in the mole ratio of 2:1 during two weeks at 150°C leads predominantly to tetramethylammonium cyclotriphosphate 9 and, as a consequence of the cleavage of trimethylamine and dimethyl ether, to small amounts of an ultraphosphate 15, which also contains cyclotriphosphate rings. 15 can be hydrolysed and neutralized with tetramethylammoniumhydroxide to yield pure 9 in the form of its trihydrate.
    Notes: Die beiden Titelverbindungen 5 und 6 reagieren miteinander im Molverhältnis 2:1 bei Temperaturen um 150°C im Verlaufe zweier Wochen im wesentlichen zum Tetramethylammonium-Salz der Cyclotriphosphorsäure 9 und durch Abspaltung von Trimethylamin und Dimethylether unter Bildung geringer Mengen eines Ultraphosphats 15, das ebenfalls Cyclotriphosphatringe enthält. Nach Hydrolyse und Neutralisation mittels Tetramethylammoniumhydroxids kann reines 9 in Form des Trihydrats isoliert werden.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845160921
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  • 2
    Electronic Resource
    Electronic Resource
    Strukturchemie titan-organischer Verbindungen: Die Struktur von [(π-C5H5)2 Ti(NO3)]2O (1981)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 479 (1981), S. 113-118 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structural Chemistry of Organotitanium Compounds: Structure of [(π-C5H5)2Ti(NO3)]2OCareful hydrolysis of (π-C5H5)2Ti(NO3)2 in tetrahydrofuran yields crystals of [(π-C5H5)2Ti(NO3)]2O (A). Crystal data of A: monoclinic, space group P21/c; lattice constants: a = 12.656(4), b = 10.181(5), c = 16.197(3) Å, ß = 93.57(3)º, Z = 4. As an X-ray analysis shows, the NO3 groups act as monodentate ligands with Ti—O distances of 2.085 and 2.059 Å. The ligands are arranged in a nearly tetrahedral way around the Ti atoms. The bond angle at the bridging O atom is 171.8º.
    Notes: Bei der vorsichtigen Hydrolyse von (π-C5H5)2Ti(NO3)2 in Tetrahydrofuran entsteht der Zweikernkomplex [(π-C5H5)2Ti(NO3)]2O (A) Kristalldaten von A: monoklin, Raumgruppe P21/c; Gitterkonstanten: a = 12,656(4), b = 10,181(5), c = 16,197(3) Å, ß = 93,57(3)º und Z = 4. Eine Röntgenstrukturanalyse ergibt, daß die Nitratgruppen als einzähnige Liganden mit Ti—O-Abständen von 2,085 und 2,059 Å fungieren. Die Ti-Atome weisen eine annähernd tetraedrische Koordination auf. Der Winkel am Brücken-O-Atom beträgt 171,8º.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19814790813
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  • 3
    Electronic Resource
    Electronic Resource
    Ein Titan(IV)-Komplex mit zwei koordinativ gebundenen Wassermolekülen: [(π-C5H5)2 Ti(H2O)2](NO3)2 (1981)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 476 (1981), S. 62-68 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Titanium (IV) Complex with Two Coordinatively Bonded Water Molecules: [(π-C5H5)2Ti(H2O)2](NO3)2(π-C5H5)2Ti(NO3)2 and H2O react in acetone to form the diaquo complex [(π-C5H5)2-Ti(H2O)2](NO3)2 (A). An X-ray analysis shows the titanium atom to be nearly tetrahedrally coordinated. Mean values of distances: Ti—O 2.01 Å, Ti—Z 2.03 Å (Z = center of ring); angles: O—Ti—O 92.7°, Z—Ti—Z 133.6°. Anions and cations are joined by hydrogen bonds to form strands that run in the direction of the crystallographic a axis. A crystallizes in the orthorhombic space group Pnma with Z = 4 and lattice parameters at - 100°C a = 7.601(2), b = 13.458(4) and c = 13.139(4) Å.
    Notes: (π-C5H5)2Ti(NO3)2 reagiert mit Wasser in Aceton unter Bildung des Diaquokomplexes [(π-C5H5)2Ti(H2O)2](NO3)2 (A). Eine Röntgenstrukturanalyse ergibt, daß das Ti-Atom eine annähernd tetraedrische Koordination besitzt. Mittelwerte der Abstände: Ti—O 2,01 Å, Ti—Z 2,03 Å (Z = Ringzentrum); Winkel: O—Ti—O 92, 7°, Z—Ti—Z 133,6°. Die Anionen und Kationen sind entlang der kristallographischen a-Achse durch Wasserstoffbrücken zu Strängen verknüpft. A kristallisiert in der orthorhombischen Raumgruppe Pnma mit Z = 4 und den Gitterkonstanten bei — 100°C a = 7,601(2), b = 13,458(4) und c = 13,139(4) Å.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19814760508
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  • 4
    Electronic Resource
    Electronic Resource
    Orbital interactions in “hypostrophene” and its hydro-and homo-derivatives. A photoelectron spectroscopic investigation (1980)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 113 (1980), S. 2120-2126 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Orbital-Wechselwirkungen in „Hypostrophen“, seinen Hydro- und Homo-Derivaten. Eine photoelektronenspektroskopische UntersuchungDie Analyse der ersten Banden in den He(I)-Photoelektronen(PE)-Spektren von „Hypostrophen“ (Tetracyclo[5.3.0.02,6.03,10]deca-4,8-dien, 3) sowie seiner Tetrahydro- (1), Dihydro- (2), Homo-(4) und Bishomo-Derivate (5) beruht auf der Korrelation zwischen den Spektren von 1 bis 5 sowie dem Vergleich mit den Ergebnissen von semiempirischen Rechnungen vom MINDO/3 und SPINDO/1-Typ. Die Elektronenstruktur des ersten angeregten Zustands von 3 und syn-Tricyclo[4.2.0.02,5]octadien wird im Zusammenhang mit dem Ausbleiben einer [π2s + π2s]- Reaktion diskutiert.
    Notes: Analysis of the first bands in the He(I) photoelectron spectra of “hypostrophene” (tetracyclo[5.3.0.02,6.03,10]deca-4,8-diene, 3), its tetrahydro- (1), dihydro- (2), homo- (4), and bishomo-derivative (5) has been achieved on the basis of the correlations within the series 1 to 5 with accompanying semiempirical calculations of the MINDO/3 and SPINDO/1 type. The electronic structure of the first excited states of 3 and syn-tricyclo[4.2.0.02,5]octadiene is discussed in light of their inability to undergo [π2s + π2s] ring closure.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19801130608
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  • 5
    Electronic Resource
    Electronic Resource
    Lewis-Säure-katalysierte Additionen 1,3-Alkyl-substituierter Allylchloride an Alkene (1984)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 117 (1984), S. 2555-2579 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Lewis Acid Catalysed Addition Reactions of 1,3-Alkyl Substituted Allyl Chlorides with AlkenesThe zinc chloride-ether catalysed reactions of 2-unsubstituted allyl chlorides (5) with alkenes (6) yield linear addition products (7) which may undergo two types of sequential reactions: Electrophilic additions to alkenes (allyl chloride induced polymerisation of alkenes) and allylation of the double bond in 7 by allyl chloride (alkene induced polymerisation of allyl chlorides). In this work we investigated systems where these sequential reactions can be reduced to a degree that electrophilic allylations of alkenes represent a synthetically useful method for CC-bond formation. - The addition reactions are not stereospecific but highly regioselective: alkenes are attacked in Markownikow sense and unsymmetrical allylic systems react at the less substituted allyl terminus. In two cases, [2 + 2]-cycloaddition reactions of allyl cations with alkenes are observed.
    Notes: Die Zinkchlorid-Ether-katalysierten Umsetzungen 2-unsubstituierter Allylchloride (5) mit Alkenen (6) liefern lineare Additionsprodukte (7), die zwei Arten von Folgereaktionen eingehen können: Elektrophile Additionen an Alkene (Allychlorid-induzierte Polymerisation der Alkene) und Allylierung der Doppelbindung von 7 durch Allylchlorid (Alken-induzierte Polymerisation der Allylchloride). Es wird untersucht, bei welchen Systemen diese Folgereaktionen soweit zurückgedrängt werden können, daß elektrophile Allylierungen von Alkenen eine präparativ brauchbare Methode zur CC-Verknüpfung darstellen. - Die Additionsreaktionen sind nicht stereospezifisch, zeigen jedoch hohe Regioselektivität: Alkene werden in Markownikow-Richtung angegriffen, unsymmetrische Allylsysteme am weniger substituierten Ende. In zwei Fällen werden [2 + 2]-Cycloadditionen von Allylkationen beobachtet.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19841170803
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  • 6
    Electronic Resource
    Electronic Resource
    Elektronenüberschuß-Komplexe von Cobalt und Nickel mit Cyclobutadien-Liganden: Synthese, Cyclovoltammetrie und Reaktivität (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 1589-1595 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Electron-Excess Complexes of Cobalt and Nickel with Cyclobutadiene Ligands: Syntheses, Cyclovoltammetry, and Reactivity[1]A cyclovoltammetric investigation of tetraphenylcyclobutadiene complexes [ML(C4Ph4)]+ [1: ML = NiCp; 2a: ML = Co(C6H6); 2b: ML = Co(mesitylene)] reveals a reversible reduction to paramagnetic complexes 1 and 2a,b with a 19-electron count, and a subsequent irreversible reduction to anions 1- and 2a,b- with a 20-electron shell. Preparative reduction by one equivalent of CpFe(HMB) (HMB = C6Me6) produces the novel 19-electron complexes 1 and 2b. Complex 1 can also be obtained by treatment of 1 · Br with one equivalent of CoCp2 at room temperature while reduction at -20°C with two equivalents of CoCp2 affords a novel C-C-linked adduct CpNi[μ,η3:η4-(C4Ph4-C5H5)]CoCp (5). Above -10°C a slow equilibrium between 5 and its components 1 and CoCp2 is observed with ΔH = 15 kJ/mol for the dissociation process. With an excess of the stronger reductant sodium amalgam the cations 1+ and 2a+ are reduced to give cyclobutenyl complexes ML(η3-1,2,3,endo-4-C4HPh4) [6: ML = NiCp; 7: ML = Co(C6H6)]. 1 reacts with p-nitrobenzyl bromide to give 1 Br and a p-nitrobenzyl addition product CpNi[η3-exo-4-(p-O2NC6H4CH2)-1,2,3,endo-4-C4Ph4] (11) while 2b reacts with MeI to give 2b · I and two isomeric methyl addition products (η5-1,3,5,exo-6-C6H3Me4)Co(C4Ph4)] (12) and (mes)Co(η3-exo-4-Me-1,2,3,endo-4-C4Ph4) (13). Sodium-amalgam reduction of the tetramethylcyclobutadiene cations [(arene)Co(C4Me4)]+ (4a: arene = C6H6; 4b: arene = mesitylene) affords diamagnetic dinuclear compounds of type 8-10 with C-C linkages between C4Me4/C4Me4, arene/C4Me4, and arene/arene rings, respectively.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250713
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  • 7
    Electronic Resource
    Electronic Resource
    Eine stereoselektive Synthese für Aminobicyclo[n.1.0]alkane verschiedener Ringgröße (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1209-1223 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Stereoselective Synthesis for Aminobicyclo[n.1.0]alkanes of Various Ring SizeEnaminosulfonium chlorides 8 are valuable intermediate products for synthesizing aminobicyclo-[n.1.0]alkanes of various ring size. Transformation of 8 to the fluorosulfate 9 and its reaction with succinimide (10) gives isolable cis-linked succinimido-bicycloalkanes 12 with 99 percent purity even with medium-large ring systems. The endo-morpholino configuration is assigned by temperature dependent 1H NMR spectroscopy; the structure 12f was proved by X-ray structure analysis. Reaction of 8e-g to the chloroenamines 13e-g followed by an interaction with 10 leads to the trans-bicyclic compounds 14e-g with a selectivity of 95-98%. With these syntheses the bicyclic derivatives 12 or 14 are obtained without isolation of intermediate products 8,9, or 13 from enamines 5, dimethyl sulfide, and N-chlorosuccinimide.
    Notes: Enaminosulfonium-chloride 8 sind wertvolle Zwischenprodukte zur Herstellung von Aminobicyclo[n.1.0]alkanen verschiedener Ringgröße. Nach der Überführung von 8 in das Fluorosulfat 9 werden mit Succinimid (10) die cis-verknüpften Succinimidobicyclen 12 erhalten, die auch im Bereich mittlere-größere Ringe mit über 99proz. Reinheit isolierbar sind. Die Ermittlung der endo-Morpholino-Konfiguration erfolgt durch temperaturabhängige 1H-NMR-Spektroskopie; für 12f wurde eine Röntgenstrukturanalyse durchgeführt. Reaktion von 8e-g zu den Chlorenaminen 13e-g und anschließende Umsetzung mit 10 führt zu den trans-Bicyclen 14e-g in einer Selektivität von 95-98%. Bei diesen Synthesen werden die Verbindungen 12 oder 14 ohne Isolierung von Zwischenprodukten 8,9 oder 13 aus Enaminen 5, Dimethylsulfid und N-Chlorsuccinimid erhalten.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150336
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  • 8
    Electronic Resource
    Electronic Resource
    Synthese von 1,2,3,3,6,6-Hexamethyl-1-cyclohexen - Eine Umlagerungskaskade von C12H23+-Kationen (1983)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 116 (1983), S. 3624-3630 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of 1,2,3,3,6,6-Hexamethyl-l-cyclohexene - A Cascade of C12H+ Carbenium Ion Rearrangements6-Chloro-2,6,7,7-tetramethyl-2-octene (4), prepared via prenyl chloride addition to 2,3,3-trimethyl-1-butene, at room temperature undergoes a zinc chloride/hydrogen chloride-catalysed cyclocondensation to yield 1,2,3,3,6,6-hexamethyl-1-cyclohexene (1). The reaction mechanism is elucidated by isolation of intermediate five-membered carbocycles and by force field calculations.
    Notes: 6-Chlor-2,6,7,7-tetramethyl-2-octen (4), das Prenylchlorid-Additionsprodukt an 2,3,3-Trimethyl-1-buten, geht bei Raumtemperatur in Gegenwart von Zinkchlorid und Chlorwasserstoff eine Cyclokondensation unter Bildung von 1,2,3,3,6,6-Hexamethyl-1-cyclohexen (1) ein. Der Reaktionsmechanismus wird durch die Isolierung intermediär auftretender fünfgliedriger Ringe und durch Kraftfeldrechnungen aufgeklärt.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19831161111
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  • 9
    Electronic Resource
    Electronic Resource
    Oxidative Trimerisierung von Alkinylgruppen an Trimethylphosphan-Palladium-Komplexen (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 9-14 
    Details
    ISSN: 0009-2940
    Keywords: Alkynyl groups ; Palladium, trimethylphosphane complexes ; Trimerization, oxidative ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Oxidative Trimerization of Alkynyl Groups at Trimethylphosphane Palladium ComplexesAlkynylpalladium halides trans-PdX (C ≡ CR)(PMe3)2 [1, 2, 4, X = Cl, R = SiMe3, (CH2)2CH3, (CH2)5CH3; 3, X = Br, R = (CH2)2CH3] were synthesized by routine methods, while further examples of the series trans-PdX (C ≡ CR)(PMe3)2 [5, 7, 8, 10, X = Br, R = SiMe3, CMe3, (CH2)2CH3, Ph; 7, 9, 11, X = I, R = SiMe3, SiPh3, OEt] and trans-PdX (C ≡ CR)(PPh3)2 (12-14, X=I, R=SiMe3, CMe3, CH2OH) were obtained by oxidative addition of 1-halogeno-1-alkynes to PdL4 (L=PMe3, PPh3). Just above the melting point or decomposition point 5-7 are transformed by oxidative trimerization of the alkynyl groups to give enediynyl complexes trans-PdX[C(C ≡ CR)=C(C ≡ CR)R](PMe3)2 (15, 16, R=SiMe3, X=Br, I; 17, X=Br, R=CMe3). According to an X-ray structure analysis 17 has E configuration.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250103
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  • 10
    Electronic Resource
    Electronic Resource
    Zur Beweglichkeit im Ionenpaar bei der aromatischen Umlagerung von O-Sulfonyl-N-phenylhydroxylaminen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2865-2871 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Internal Mobility in the Ion Pairs during Aromatic Rearrangement of O-Sulfonyl-N-phenylhydroxylaminesIn the rearrangement of O-alkyl- or O-arylsulfonyl-N-benzoyl-N-phenylhydroxylamines 3 to aminophenols 4, the internal mobility in the ion pair intermediates depends both on the size of the alkyl groups and on the interaction with the protic solvent, as was shown by 18O labeled educts.
    Notes: Bei der Umlagerung von O-Alkyl- bzw. O-Arylsulfonyl-N-benzoyl-N-phenylhydroxylaminen 3 in Aminophenole 4 wird durch 18O-Indizierung gezeigt, daß die Beweglichkeit in den intermediär gebildeten Ionenpaaren durch große Alkylreste sowie durch Wechselwirkung mit einem protischen Lösungsmittel in typischer Weise verändert wird.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150817
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