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  • 1982  (25)
  • 1
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Carben-Komplexe, CXXII. Kinetische und mechanistische Untersuchungen von übergangsmetall-Komplex-Reaktionen, XII. Pentacarbonyl[diethylamino(triphenylplumbyl)carben]chrom und trans-Tetracarbonyl(diethylaminocarbin)(triphenyl-plumbyl)chrom: Präparative Untersuchungen und Kinetik der C,Cr-Wanderung von PbPh3 (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2707-2713 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Carbene Complexes, CXXII. Kinetic and Mechanistic Investigations of Transition Metal Complex Reaction, XII. Pentacarbonyl[diethylamino(triphenylplumbyl)carbene]chromium and trans-Tetracarbonyl(diethylaminocarbyne)(triphenylplumbyl)chromium: Preparative Investigations and Kinetics of the C,Cr-Migration of PbPh3Pentacarbonyl(diethylaminocarbyne)chromium tetrafluoroborate, [(CO)5CrCNEt2]BF4 (2), reacts with lithium triphenylplumbate, LiPbPh3 (3), with addition of the plumbate anion to the carbyne carbon atom to give pentacarbonyl[diethylamino(triphenylplumbyl)carbene]chromium, (CO)5-Cr[C(PbPh3)NEt2] (4). Already at room temperature, the complex 4 rearranges with CO-elimination and C,Cr-migration of PbPh3 to give trans-tetracarbonyl(diethylaminocarbyne)(triphenylplumbyl)chromium, trans-(Ph3Pb)(CO)4CrNEt2 (5). The rearrangement follows a first-order rate law (ΔH≠ = 103 kJmol-1; ΔS≠ = 40 Jmol-1, K-1, in 1,1,2-trichloroethane). The compounds 4 und 5 were characterized by analytical and spectroscopic means.
    Notes: Pentacarbonyl(diethylaminocarbin)chrom-tetrafluoroborat, [(CO)5CrCNEt2]BF4 (2), reagiert mit Lithium-triphenylplumbat, LiPbPh3 (3), unter Addition des Plumbat-Anions an das Carbinkohlenstoffatom und Bildung von Pentacarbonyl[diethylamino(triphenylplumbyl)carben]chrom, (CO)5Cr[C(PbPh3)NEt2] (4). Bereits bei Raumtemperatur lagert sich der Komplex 4 unter CO-Abspaltung und C,Cr-Wanderung von PbPh3 nach einem Geschwindigkeitsgesetz erster Ordnung (ΔH≠ = 103 kJmol-1, ΔS≠ = 40 Jmol-1, K-1, in 1,1,2-Trichlorethan) zu trans-Tetracarbonyl-(diethylaminocarbin)(triphenylplumbyl)chrom, trans-(Ph3Pb)(CO)4CrCNEt2 (5), um. Die Verbindungen 4 und 5 wurden analytisch und spektroskopisch gesichert.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19821150804
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  • 2
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Carben-Komplexe, CXXIV. Ein- und zweikernige Biscarbenkomplexe von Chrom, Molybdän und Wolfram und ihre Umsetzung mit Bortrihalogeniden (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 2951-2964 
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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 Carbene Complexes, CXXIV. Mono- and Binuclear Biscarbene Complexes of Chromium, Molybdenum, and Tungsten and their Reaction with Boron TrihalidesThe reaction of p-phenylenedilithium with hexacarbonylchromium and -tungsten and subsequent alkylation by triethyloxonium tetrafluoroborate yields μ-[p-phenylenebis[(ethoxy)carbene]]-bis-(pentacarbonylmetal) complexes (CO)5MC(OEt)-p-C6H4-(OEt)CM(CO)5 (M = Cr (3a), W (3b)) as well as the mononuclear carbene complexes 4a and 4b. The analogous reaction of o-phenylenedilithium with metalhexacarbonyls of the VI. subgroup affords the expected mononuclear 1,4-chelated biscarbene complexes (M = Cr (5a), Mo (5b), W (5c)), while 1,2-dilithio-1,2-diphenylethane gives a mixture of mononuclear (M = Cr (6a), W (6b)) and binuclear (CO)5MC(OEt)CH(Ph)CH(Ph)-(OEt)CM(CO)5 (M = Cr (7a), W (7b)) biscarbene complexes. The aminolysis of 5a - c with dimethylamine leads to cis-tetracarbonyl[o-phenylenebis[(dimethylamino)carbene]] compounds of chromium, molybdenum, and tungsten (8a - c). 3a, b and 4a, b react with boron trihalides BX3 to form the corresponding trans-halogenocarbyne complexes 9a, b and 10a - c. Properties, spectra, and the results of an X-ray structure analysis of 9b are reported.
    Notes: Die Umsetzung von p-Phenylendilithium mit Hexacarbonylchrom und -wolfram und anschließende Alkylierung mit Triethyloxonium-tetrafluoroborat ergibt μ-[p-Phenylenbis[(ethoxy)carben]]-bis(pentacarbonylmetall)-Komplexe (CO)5MC(OEt)-p-C6H4-(OEt)CM(CO)5 (M = Cr (3a), W (3b)), sowie die einkernigen Carbenkomplexe 4a und 4b. Die analoge Reaktion von o-Phenylendilithium mit Metallhexacarbonylen der VI. Nebengruppe ergibt die erwarteten einkernigen, 1,4-chelatisierten Biscarbenkomplexe (M = Cr (5a), Mo (5b), W (5c)), während 1,2-Dilithio-1,2-diphenylethan ein Gemisch von einkernigen (M = Cr (6a), W (6b)) und zweikernigen (CO)5MC(OEt)CH(Ph)CH(Ph)(OEt)CM(CO)5 (M = Cr (7a), W (7b)) Biscarben-Komplexen liefert. Die Aminolyse von 5a-c mit Dimethylamin führt zu cis-Tetracarbonyl[o-phenylenbis[(dimethylamino)carben]]-Verbindungen von Chrom, Molybdän und Wolfram (8a-c-). 3a, b und 4a, b reagieren mit Bortrihalogeniden BX3 unter Bildung der entsprechenden trans-Halogenocarbin-Komplexe 9a, b und 10a-c. Eigenschaften, Spektren und die Ergebnisse einer Röntgenstrukturuntersuchung an 9b werden beschrieben.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150903
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  • 3
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    Electronic Resource
    Absolute Konfiguration von Antheraxanthin, «cis-Antheraxantliirt» und der diastereomeren Mutatoxanthine (1982)
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 65 (1982), S. 2198-2211 
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    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Absolute Configuration of Antheraxanthin, ‘cis-Aritheraxanthin’ and of the Stereoisomeric MutatdxanthinsThe assignement of structure 2 to antheraxanthin (all-E)-(3 S, 5 R, 6 S, 3′ R)-5,6-epoxy-5,6-dihydro-β,β-carotene-3,3′-diol and of 1 to ‘cis-antheraxanthin’ (9Z)-(3 S, 5 R, 6 S, 3′ R)-5,6-epoxy-5,6-dihydro-β,β-carotene-3,3′-diol is based on chemical correlation with (3 R, 3′ R)-zeaxanthin and extensive 1H-NMR. measurements at 400 MHz. ‘Semisynthetic antheraxanthin’ ( = ‘antheraxanthin B’) has structure 6. For the first time the so-called ‘mutatoxanthin’, a known rearrangement product of either 1 or 2, has been separated into pure and crystalline C(8)-epimers (epimer A of m.p. 213° and epimer B of m.p. 159°). Their structures were assigned by spectroscopical and chiroptical correlations with flavoxanthin and chrysanthemaxanthin. Epimer A is (3 S, 5 R, 8 S, 3′ R)-5,8-epoxy-5,8-dihydro-β,β-carotene-3,3′-diol (4; = (8 S)mutatoxanthin) and epimer B is (3 S, 5 R, 8 R, 3′ R)-5,8-epoxy-5,8-dihydro-β,β-carotene-3,3′-diol (3; = (8 R)-mutatoxanthin). The carotenoids 1-4 have a widespread occurrence in plants. We also describe their separation by HPLC. techniques. CD. spectra measured at room temperature and at - 180° are presented for 1-4 and 6. Antheraxanthin (2) and (9Z)-antheraxanthin (1) exhibit a typical conservative CD. The CD. Spectra also allow an easy differentiation of 6 from its epimer 2. The isomeric (9Z)-antheraxanthin (1) shows the expected inversion of the CD. curve in the UV. range. The CD. spectra of the epimeric mutatoxanthins 3 and 4 (β end group) are dissimilar to those of flavoxanthin/chrysanthemaxanthin (ε end group). They allow an easy differentiation of the C (8)-epimers.
    Additional Material: 10 Ill.
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    URL: http://dx.doi.org/10.1002/hlca.19820650725
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  • 4
    Electronic Resource
    Electronic Resource
    Übergangsmetall-Carbin-Komplexe, LXVIII. Synthese und Struktur neuartiger zweikerniger Biscarbin-Komplexe des Chroms, Molybdäns und Wolframs mit verbrückenden Phenylthio-, Arylseleno-, Halogeno- und Pseudohalogeno-Liganden (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3152-3166 
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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, LXVIII. Synthesis and Structure of Novel Binuclear Biscarbyne Complexes of Chromium, Molybdenum, and Tungsten with Bridging Phenylthio-, Arylseleno-, Halogeno-, and Pseudohalogeno LigandsPentacarbonyl[(diethylamino)(ethoxy)carbene]molybdenum (1) reacts with boron trifluoride to give a very unstable product which is supposed to be pentacarbonyl[(diethylamino)carbyne]-molybdenum tetrafluoroborate (2). Low temperature reaction of 2 with bromide, iodide, and thiocyanate yields the neutral trans-substituted carbyne complexes trans-X(CO)4MoCNEt2 (4a-c) [X = Br (a), I (b), SCN (c)] cyanate and 4-(trifluoromethyl)phenylselenolate afford the compounds (μ-X)2[(CO)3MoCNEt2]2 (5d, f) [X = OCN (d), 4-CF3C6H4Se (f)] which are members of a new class of binuclear biscarbyne complexes. Analogues 5a-c, g-l are prepared from the carbyne complexes trans-X(CO)4MCNR2 (4a-c, g-l) on warming in solution. The corresponding complex 5e (X = N3, M = W, R = C2H5) is obtained by the reaction of pentacarbonyl[(diethylamino)carbyne]tungsten tetrafluoroborate (6) with azide. The structures of 5b, d, e, g are ensured by X-ray analyses.
    Notes: Pentacarbonyl[(diethylamino)(ethoxy)carben]molybdän (1) reagiert mit Bortrifluorid zu einem sehr instabilen Produkt, bei dem es sich vermutlich um Pentacarbonyl[(diethylamino)carbin]-molybdän-tetrafluroborat (2) handelt. Wird 2 bei tiefer Temperatur mit Bromid, Iodid und Thiocyanat umgesetzt, erhält man die neutralen trans-substituierten Carbinkomplexe trans-X(CO)4MoCNEt2 (4a-c) [X = Br (a), I (b), SCN (c)] demgegenüber ergeben Cyanat und 4-(Trifluormethyl)phenylselenolat die Verbindungen (μ-X)2[(CO)3MoCNEt2]2 (5d, f) [X = OCN (d), 4-CF3C6H4Se (f)] als Vertreter einer neuen Klasse von zweikernigen Biscarbin-Komplexen. Die dazu analogen Verbindungen 5a-c, g--l werden dargestellt, indem man die Carbinkomplexe trans-X(CO)4MCNR2 (4a-c, g-l) in Lösung aufwärmt. Der entsprechende Komplex 5e (X = N3, M = W, R = C2H5) wird bei der Umsetzung von Pentacarbonyl[(diethylamino)carbin]-wolfram-tetrafluoroborat (6) mit Azid erhalten. Der Aufbau von 5b, d, e, g ist durch Röntgenstrukturanalysen gesichert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150920
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  • 5
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    Kinetische und mechanistische Untersuchungen von Übergangsmetallkomplex-Reaktionen, XI. Reaktionen von Komplexliganden, XXII. Kinetik und Mechanismus der Bildung von Tricarbonyl-(naphthol)chrom-Komplexen aus Pentacarbonyl-[(methoxy)(phenyl)carben]chrom(0) und Alkinen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1355-1362 
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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, XI. Reactions of Complex Ligands, XXII. Kinetic and Mechanism of the Formation of Tricarbonyl(naphthol)chromium Complexes from Pentacarbonyl[(methoxy)(phenyl)carbene]chromium(0) and AlkynesPentacarbonyl[(methoxy)(phenyl)carbene]chromium(0), (CO)5Cr[C(Ph)OMe] (1), reacts with arylalkynes p-R1C6H4—C≡C—R2 (R1 = H, Me; R2 = Ph, 4-C6H4CF3, Me) (2a-e) with elimination of CO to give substituted tricarbonyl(1-naphthol)chromium complexes (3a-e, 4a-d) in dibutyl ether by the following rate law: -d[1]/dt = {k1k2[2]/(k-1[CO] + k2[2])} [1]. The activation parameters for the CO-elimination reaction are: ΔH± = 108 ± 2 kJ mol-1, ΔS± = 26 ± 6 J mol-1 K-1. The reaction rate increases with increasing electron density within the triple bond of 2a-e. The results are discussed on the basis of a dissociative mechanism.
    Notes: Pentacarbonyl[(methoxy)(phenyl)carben]chrom(0), (CO)5Cr[C(Ph)OMe] (1), reagiert mit den Arylalkinen p-R1C6H4—C≡C—R2 (R1 = H, Me; R2 = Ph, 4-C6H4CF3, Me) (2a-e) unter CO-Abspaltung zu substituierten Tricarbonyl(1-naphthol)chrom-Komplexen (3a-e, 4a-d) in Dibutylether nach folgendem Geschwindigkeitsgesetz: —d[1]/dt = {k1k2[2]/(k-1[CO] + k2[2])}[1]. Die Aktivierungsparameter für die CO-Abspaltung sind: ΔH± = 108 ± 2 kJ mol-1, ΔS± = 26 ± 6 J mol-1 K-1. Mit steigender Elektronendichte in der Dreifachbindung von 2a-e nimmt die Geschwindigkeit der Umsetzung zu. Die Ergebnisse werden auf der Grundlage eines dissoziativen Mechanismus diskutiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150412
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  • 6
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    Thioketon-Komplexe durch Insertion des Schwefels von Organylisothiocyanaten in die Metall-Carbenkohlenstoff-Bindung (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 1349-1354 
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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: Thioketone Complexes via Insertion of Sulfur from Organyl Isothiocyanates into the Metal-Carbene Bond(Arylphenylcarbene)pentacarbonyltungsten complexes, (CO)5W[C(p-C6H4R)(C6H5)] (1) [R = H (a), OMe (b), Me (c), Br (d), CF3 (e)], react with organyl isothiocyanates, R′—N=C=S (2) [R = Me (a), Et (b), Ph (3c)], inserting sulfur from 2 into the metal-carbene bond to give (arylphenyl thioketone)pentacarbonyltungsten complexes, (CO)5W[S=C(p-C6H4R)(C6H5)] (3). The compounds 3 were characterized by spectroscopic means.
    Notes: (Arylphenylcarben)pentacarbonylwolfram-Komplexe, (CO)5W[C(p-C6H4R)(C6H5)] (1) [R = H (a), OMe (b), Me (c), Br (d), CF3 (e)], reagieren mit Organyl-isothiocyanaten, R′—N=C=S (2) [R′ = Me (a), Et (b), Ph (c)], unter Insertion des Schwefels von 2 in die Metall-Carbenkohlenstoff-Bindung und Bildung von [(Aryl)(phenyl)thioketon]pentacarbonylwolfram-Komplexen, (CO)5W[S=C(p-C6H4R)(C6H5)] (3). Die Verbindungen 3 wurden mit Hilfe von spektroskopischen Methoden charakterisiert.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821150411
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  • 7
    Electronic Resource
    Electronic Resource
    Neue Reagentien, XVIII. (Lithiomethyl)diphenylarsanoxid; Synthese und Anwendung zur indirekten nucleophilen Halomethylierung (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 645-653 
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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: New Reagents, XVIII. (Lithiomethyl)diphenylarsane Oxide; Synthesis and Application for the Indirect Nucleophilic HalomethylationDue to its ready accessibility and high nucleophilicity (lithiomethyl)diphenylarsane oxide (2b) is a favorable reagent for the synthesis of many organoarsenic compounds. In organic synthesis it is recommendable as a reagent for indirect nucleophilic halomethylations (Hal = Cl, Br, I).
    Notes: (Lithiomethyl)diphenylarsanoxid (2b) ist wegen seiner bequemen Zugänglichkeit und hohen Nucleophilie ein günstiges Reagens zur Darstellung zahlreicher Organoarsenverbindungen. In der organischen Synthese ist es als Reagens für indirekte nucleophile Halomethylierungen (Hal = Cl, Br, I) empfehlenswert.
    Additional Material: 4 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19821150224
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  • 8
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    Electronic Resource
    Übergangsmetall-Carbin-Komplexe, LXVII. Kationische Carbin-Komplexe des Wolframs  -  Synthese, Struktur und Reaktionsverhalten gegenüber Nucleophilen (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3141-3151 
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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, LXVII. Cationic Carbyne Complexes of Tungsten - Synthesis, Structure, and Reaction with NucleophilesPentacarbonyl[(diethylamino)(ethoxy)carbene]tungsten (1) reacts with boron trifluoride to give the unstable cationic carbyne complex pentacarbonyl[(diethylamino)carbyne]tungsten tetrafluoroborate (2a). Replacing the BF4- anion by SbX6- yields the more stable compounds [(CO)5WCNEt2]SbX6 [2c (X = F) and 2d (X = Cl)]. The X-ray structure determination of 2d shows that there are at most charge transfer-like anion-cation interactions in the crystal. Complex 2a shows two different types of reaction with nucleophiles X-: rearrangement with CO-elimination gives trans-BF4(CO)4WCNEt2 (3a) even at low temperatures. The neutral carbyne complexes trans-X(CO)4WCNEt2 [4a-e; X = CN (a), NCO (b), NCS (c), NCSe (d), SC6H5 (e)] are then formed by nucleophilic substitution of BF4- by X- on 3a. In case of X- = As(C6H5)2- only nucleophilic addition to the carbyne carbon atom of 2a is observed to afford pentacarbonyl[(diethylamino)(diphenylarsino)carbene]tungsten (5). Complex 2d reacts with X- (X = SC6H5, OC6H5) at low temperature - or without X- on warming - to give trans-Cl(CO)4WCNEt2 (4f).
    Notes: Pentacarbonyl[(diethylamino)(ethoxy)carben]wolfram (1) reagiert mit Bortrifluorid zum instabilen kationischen Carbinkomplex Pentacarbonyl[(diethylamino)carbin]wolfram-tetrafluoroborat (2a). Ersetzt man das BF4--Anion durch SbX6-, erhält man die stabileren Verbindungen [(CO)5WCNEt2]SbX6[2c (X = F) und 2d (X = Cl)]. Eine von 2d durchgeführte Röntgenstrukturanalyse zeigt, daß im Kristall höchstens Charge-Transfer-artige Kation-Anion-Wechselwirkungen vorliegen. Gegenüber Nucleophilen X- zeigt Komplex 2a zwei verschiedene Reaktionsmöglichkeiten: die bereits bei tiefen Temperaturen unter CO-Abspaltung erfolgende teilweise Umlagerung von 2a zu trans-BF4(CO)4WCNEt2 (3a) führt nach nucleophiler Substitution von BF4- durch X- in 3a zu den neutralen Carbinkomplexen trans-X(CO)4WCNEt2 [4a-e; X = CN (a), NCO (b), NCS (c), NCSe (d), SC6H5 (e)]. Im Fall von X- = As(C6H5)2- beobachtet man ausschließlich Addition des Nucleophils an das Carbin-Kohlenstoffatom von 2a und Bildung von Pentacarbonyl[(diethylamino)(diphenylarsino)carben]wolfram (5). Komplex 2d ergibt durch Umsetzung mit X- (X = SC6H5, OC6H5) bei tiefen Temperaturen - beim Erwärmen auch in Abwesenheit von X- - stets trans-Cl(CO)4WCNEt2 (4f).
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19821150919
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  • 9
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    Übergangsmetall-Carben-Komplexe, CXXV. Sekundäre ein- und zweikernige Alkoxy- und Dimethylamino-carben-Komplexe des Rheniums (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3851-3859 
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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 Carbene Complexes, CXXV. Secondary Mono- and Dinuclear Alkoxy- and Dimethylaminocarbene Complexes of RheniumThe reaction of cationic silylcarbone complexes of rhenium [π-C5H5(CO)2ReCSi(C6H5)3]BF4 (1) and ax—[(CO)9Re2CSi(C6H5)3]AlX4 (X = Cl 6, X = Br 7) with alcohols (methanol, ethanol, 2-propanol, tert-butylalcohol) or dimethylamine yields not only the expected alkoxy(silyl)carbene- and dimethylamino(silyl)carbene complexes (2,4) but also secondary alkoxy- and dimethylamino- carbene complexes (3, 5, 8 - 11, 14). In case of the reactions of 6 and 7, halogen(silyl)carbene complexes (12, 13) are isolated as intermediates. Properties, spectroscopic results, and the X-ray structure analysis of eq-(CO)9Re2C(H)OCH3 (8) are reported.
    Notes: Die kationischen Silylcarbin-Komplexe des Rheniums [π-C5H5(CO)2ReCSi(C6H5)3]BF4 (1) und ax—[(CO)9Re2CSi(C6H5)3]AlX4 (X = Cl 6, X = Br 7) reagieren mit Alkoholen (Methanol, Ethanol, 2-Propanol, tert-Butylalkohol) oder Dimethylamin nicht nur zu den erwarteten Alkoxy-(silyl)carben- bzw. Dimethylamino(silyl)carben-Komplexen (2, 4), sondern auch zu sekundären Alkoxy- und Dimethylaminocarben-Komplexen (3, 5, 8 - 11, 14). Als Zwischenprodukte lassen sich bei der Umsetzung von 6 und 7 Halogen(silyl)carben-Komplexe (12 und 13) isolieren. Eigenschaften und spektroskopische Daten sowie die Röntgenstrukturanalyse von eq-(CO)9Re2C(H)—OCH3 (8) werden beschrieben.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19821151216
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  • 10
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    Unterschiedliche [4 + 2]-Cycloaddukte aus 7,7-Difluor- und 7,7-Dialkoxy-1,3,5-cycloheptatrienen mit 4-Phenyl-1,2,4-triazolin-3,5-dion (1982)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 115 (1982), S. 3427-3435 
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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: [4 + 2] Cycloadducts with Alternate Structure from 7,7-Difluoro- and 7,7-Dialkoxy-1,3,5-cycloheptatrienes and 4-Phenyl-1,2,4-triazoline-3,5-dioneWith 4-phenyl-1,2,4-triazoline-3,5-dione (PTAD), 7,7-difluoro-, 7,7-dimethoxy-, 7,7-(trimethylenedioxy)- and 7,7-(ethylenedioxy)-1,3,5-cycloheptatriene (1c-f) form 1:1 cycloadducts of different structure. For the cycloadducts from 1d, e and cycloheptatriene itself, 13C and 1H NMR spectra establish a structure formally derived from the norcaradiene valence tautomer (2a, d, e) by [4 + 2] cycloaddition (NCD-type, 4). 1c, f and tropone, on the other hand, undergo [4 + 2] cycloaddition at C-1/C-4 of the cycloheptatriene skeleton, yielding adducts of the CHT-type 3.
    Notes: 4-Phenyl-1,2,4-triazolin-3,5-dion (PTAD) bildet mit 7,7-Difluor-, 7,7-Dimethoxy-, 7,7-(Trimethylendioxy)- und 7,7-(Ethylendioxy)-1,3,5-cycloheptatrien (1c-f) 1:1-Cycloaddukte unterschiedlicher Struktur. Nach 13C- und 1H-NMR-Spektren besitzen die Cycloaddukte aus 1d, e und dem unsubstituierten Cycloheptatrien eine Struktur, die sich vom Norcaradien-Valenztautomeren (2a, d, e) durch [4 + 2]-Cycloaddition ableiten läßt (NCD-Typ, 4). Bei 1c, f und beim Tropon dagegen erfolgt [4 + 2]-Cycloaddition an C-1/C-4 des Cycloheptatrien-Skeletts: es entstehen Addukte vom CHT-Typ 3.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19821151019
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