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  • 2,4-Bis(di-tert-butylphosphino)-1,2,3,4-tetraphosphabicyclo[1.1.0]butane P4(PtBu2)2  (1)
  • One-pot reactions of tri-t-butoxychlorosilane, K-t-butanolate and substituted anilines. Crystal structure analyses of N-(tri-t-butoxysilyl)-aniline, C18H33NO3Si  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Der thermische Zerfall des tBu2P—P=P(Me)tBu2Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1769-1773 
    Details
    ISSN: 0044-2313
    Keywords: Phosphinophosphinidene-phosphorane tBu2P—P=P(Me)tBu2 ; formation of tBu2PMe and the phosphinophosphinidene tBu2P—P ; 2,4-Bis(di-tert-butylphosphino)-1,2,3,4-tetraphosphabicyclo[1.1.0]butane P4(PtBu2)2 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Thermal Decomposition of tBu2P—P=P(Me)tBu2The thermal decomposition of tBu2P—P=P(Me)tBu2 2 in C6H6 at 20°C is detectable after 10 h; tBu2PMe, (tBu2P)2PH and small amounts of the cyclotetraphosphanes P4(PtBu2)4 and P4(PtBu2)2 are formed. At 70°C (14 h) 83% of 2 are decomposed, and even 96% after 74 h. The main products are tBu2PMe (68%) and P4(PtBu2)4 (20%). With 2,3-dimethyl-1,3-butadiene as a trapping reagent tBu2PMe (62%) is still the main product, however, P4(PtBu2)4 is no longer found, but 1,2-bis(di-tert-butylphosphino)-4,5-dimethyl-1,2-diphosphacyclohexene-4 (22%) is formed instead. Also with cyclohexene tBu2PMe (78%) remains the major product besides P4(PtBu2)4 (9%) and small amounts of the trapping product 7-di-tert-butylphosphino-7-phosphabicyclo[4.1.0]heptane. Thus, the thermal decomposition of 2 at 70°C proceeds very similar to that of tBu2P—P=P(Br)tBu2 at -30°C and starts yielding and the phosphinophosphinidene tBu2P—P. In CH2Cl2 the decomposition of 2 includes the chlorination of the ylidic molecule.
    Notes: Die thermische Zersetzung von tBu2P—P=P(Me)tBu2 2 in C6H6 ist bei 20°C nach 10 h nachweisbar, wobei tBu2PMe, (tBu2P)2PH und geringe Mengen der Cyclotetraphosphane P4(PtBu2)4 und von P4(PtBu2)2 entstehen. Bei 70°C (14 h) sind 83% von 2 zerfallen, nach 75 h 97%. Hauptprodukte sind tBu2PMe (68%) und P4(PtBu2)4 (20%). In Anwesenheit des Abfangreagenzes 2,3-Dimethyl-1,3-butadien bleibt tBu2PMe (62%) Hauptprodukt, doch P4(PtBu2)4 wird nicht mehr gebildet, sondern es entsteht 1,2-Bis(di-tert-butylphosphino)-4,5-dimethyl-1,2-diphosphacyclohexen-4 (22%). Mit Cyclohexen ist tBu2PMe Hauptprodukt (78%) neben P4(PtBu2)4 (9%) und geringen Anteilen des Abfangproduktes 7-Di-tert-butylphosphino-7-phosphabicyclo[4.1.0]heptan. Damit entspricht der Zerfall von 2 bei 70°C weitgehend dem des tBu2P—P=P(Br)tBu2 bei -30°C und beginnt mit der Bildung von tBu2PMe und des Phosphinophosphinidens tBu2P—P. In CH2Cl2 läuft die Zersetzung von 2 über die Chlorierung und Zersetzung des Ylidgerüstes.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231118
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  • 2
    Electronic Resource
    Electronic Resource
    Darstellung und Strukturen einiger N-(Tri-t-butoxysilyl)anilin-Derivate (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 377-384 
    Details
    ISSN: 0044-2313
    Keywords: One-pot reactions of tri-t-butoxychlorosilane, K-t-butanolate and substituted anilines. Crystal structure analyses of N-(tri-t-butoxysilyl)-aniline, C18H33NO3Si ; N-(tri-t-butoxysilyl)-p-nitroaniline, C18H32N2O5Si ; N-Methyl-(N-tri-t-butoxysilyl)-p-nitroaniline C19H34N2O5Si ; N-(tri-t-butoxysilyl)-p-cyanoaniline, C19H32N2O3Si ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structures of N-(tri-t-butoxysilyl)aniline CompoundsPara-substituted N-(tri-t-butoxysilyl)anilines (t-BuO)3SiNRC4H4X-p, R = H, CH3, with substituents of high electron affinity (X = CN, NO2) were prepared by a one-pot reaction of tri-t-butoxychlorsilane, potassium t-butanolate and substituted anilines. Corresponding compounds with substituents of low electron affinity (X = OMe, H) preferably were prepared by metalation of anilines with sodium amide. Four crystal structures were determined. N-(tri-t-butoxysilyl)-p-nitro-aniline, N-methyl-(N-tri-t-butoxysilyl)-p-nitroaniline and N-(tri-t-butoxysilyl)-p-cyanoaniline crystallize at 298 K monoclinically, N-(tri-t-butoxysilyl)aniline crystallizes orthorhombically.
    Notes: Derivate des para-substituierten N-(Tri-t-butoxysilyl)anilins (t-BuO)3SiNRC6H4X-p, R = H, CH3 mit Substituenten hoher Elektronenaffinität (X = CN, NO2) wurden nach einem neuen Eintopfverfahren aus Tri-t-butoxychlorsilan, Kalium-t-butanolat und dem entsprechend substituierten Anilin dargestellt. Für Substituenten niederer Elektronenaffinität (X = OMe, H) wird die Methode der Metallierung von Anilinen mit Natriumamid bevorzugt. Vier Kristallstrukturen wurden bestimmt. N-(Tri-t-butoxysilyl)-p-nitroanilin, N-Methyl-(N-tri-t-butoxysilyl)-p-nitroanilin und N-(Tri-t-butoxysilyl)-p-cyanoanilin kristallisieren bei 298 K monoklin, N-(Tri-t-butoxysilyl)anilin kristallisiert orthorhombisch.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200230
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