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  • 1
    Electronic Resource
    Electronic Resource
    Zum Einfluß der Substituenten R = Ph, NEt2, iPr und tBu in Triphosphanen, (R2P)2P—SiMe3, und Phosphiden, Li(THF)2[(R2P)2P], auf die Bildung und Eigenschaften von Phosphinophosphiniden-PhosphoranenFrau Professor Marianne Baudler zum 75. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 935-941 
    Details
    ISSN: 0044-2313
    Keywords: Triphosphanes ; Phosphides, Phosphino-phosphinidene-phosphoranes ; 31P NMR data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Concerning the Influence of the Substituents R = Ph, NEt2, iPr, and tBu in Triphosphanes (R2P)2P—SiMe3 and Phosphides Li(THF)2[(R2P)2P] on the Formation and Properties of Phosphino-phosphinidene-phosphoranesThe triphosphanes X2P—P(SiMe3)—PY2 5, 7, 9, 11, 13 and the derived phosphides Li(THF)2[X2P—P—PY2] 6, 8, 10, 12, 14 were synthesized: 5 and 6 with X2 = iPr2 and Y2 = tBu2, 7 and 8 with X2 = Y2 = PhtBu, 9 and 10 with X2 = tBu2 and Y2 = Ph2, 11 and 12 with X2 = Y2 = Ph2, and 13 and 14 with X2 = tBu2 and Y2 = (NEt2)2.The silylated triphosphanes at -70°C in toluene with CBr4 may yield X2P—P=P(Br)Y2 and X2P—P(Br)—PY2, and the lithiated phosphides with MeCl may yield X2P—P=P(Me)Y2 and X2P—P(Me)—PY2 depending on X and Y. The bromiated product of 5 (X2 = iPr2, Y2 = tBu2) is the ylide iPr2P—P=P(Br)tBu2, and the methylated derivatives of 6 are both iPr2P—P=P(Me)tBu2, tBu2P—P=P(Me)iPr and the methylated triphosphane. Ph2P—P=P(Br)tBu2 as well as the brominated triphosphane are obtained from 9 (X2 = tBu2, Y2 = Ph2), and similarly Ph2P—P=P(Me)tBu2 and the methylated triphosphane from 10. Compound 14 (X2 = tBu2, Y2 = (NEt2)2 gives rise to the brominated ylide tBu2)P—P=P(Br) · (NEt2)2 and to the brominated triphosphane, and on methylation to tBu2P—P=P(Me)(NEt2)2 and to tBu2P—P(Me)—P · (NEt2)2 (main product). The Br substituted derivatives decompose already on warming to -30°C, while the methylated compounds are stable up to 20°C.
    Notes: Die Triphosphane X2P—P(SiMe3)—PY2 5, 7, 9, 11, 13 und die entsprechenden Phosphide 6, 8, 10, 12, 14 wurden synthetisiert, 5 und 6 mit X2 = iPr2 und Y2 = tBu2, 7 und 8 mit X2 = Y2 = PhtBu, 9 und 10 mit X2 = tBu2 und Y2 = Ph2, 11 und 12 mit X2 = Y2 = Ph2 sowie 13 und 14 mit X2 = tBu2 und Y2 = (NEt2)2.Die silylierten Triphosphane bilden mit CBr4 in Toluol bei -70°C X2P—P=P(Br)Y2 und X2P—P(Br)—PY2, die lithiierten Phosphide mit MeCl Abstand X2P—P=P(Me)Y2 und X2P—P(Me)—PY2. Der Reaktionsverlauf ist abhängig von den Gruppen X und Y. Das Bromierungsprodukt von 5 (X2 = iPr2, Y2 = tBu2) ist das Ylid iPrP—P=P(Br)tBu2, während die Methylierung des entsprechenden Phosphides 6 zu den beiden Yliden iPrP—P=P(Me)tBu2, tBu2P—P=P(Me)iPr2 und dem methylierten Triphoshan führt. Von 9 (X2 = tBu2, Y2 = Ph2) wurden sowohl Ph2P—P=P(Br)tBu2 als auch das bromierte Triphosphan gebildet, von dem entsprechenden Phosphid 10 das Ph2P—P=P(Me)tBu2 und das methylierte Triphosphan. Verbindung 14 (X2 = tBu2, Y2 = (NEt2)2) reagiert zum bromierten Ylid tBu2P—P=P(Br)(NEt2)2 und dem bromierten Triphosphan, bei Methylierung zu tBu2P—P=P(Me)(NEt2)2 und tBu2P—P(Me)—P(NEt2)2 (Hauptprodukt). Die Br-substituierten Derivate zersetzen sich bereits beim Erwärmen auf -30°C, während die methylierten bis zu 20°C beständig sind.
    Additional Material: 7 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220604
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  • 2
    Electronic Resource
    Electronic Resource
    Komplexchemie P-reicher Phosphane und Silylphosphane. XII. Bildung und Struktur von Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] und (tBu2P)2P—SiMe3Professor Kurt Dehnicke zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1564-1572 
    Details
    ISSN: 0044-2313
    Keywords: Li(THF)2[η2-(tBu2P)2P] ; Li(TMEDA)[η2-(tBu2P)2P] ; Li(THF)2[η2-(iPr2P)2P] ; Li(THF)2[η2-(Et2N)2P—P—PtBu2] ; Li(THF)2[η2-(tBu2P—P—PiPr2)] ; (tBu2P)2P—SiMe3 ; crystal structures ; 1H, 31P, 7Li-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structure of Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] and (tBu2P)2P—SiMe3The formation and crystal structures of the compounds (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA)[η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 and Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 are reported. Compounds 3-6 are formed by reacting the corresponding silylated triphosphanes with nBuLi: 2 and 3 result from (tBu2P)2P—SiMe3 1, 4 from (iPrP)2P—SiMe3, 5 from (Et2N)2P—P(SiMe3)—PtBu2 and 6 from tBu2P—P(SiMe3)—PiPr2. 1 crystallizes in the orthorhombic space group P212121 (no. 19) with a = 910.87(7) pm, b = 1132.5(1) pm, c = 2373.5(2) pm (determined at 90 K). The structure determination of 2 was performed at 293 K and 200 K, respectively. 2 crystallizes in the monoclinic space group P21/n (no. 14) with a = 1069.7(3) pm, b = 1802.5(3) pm, c = 1604.0(7) pm, β = 98.11(2)° (200 K); 3 also in P21/n (no. 14) with a = 904.3(2) pm, b = 1936.4(5) pm, c = 1653.2(3) pm, β = 94.52(1)° (200 K). 4 crystallizes monoclinically in C2/c (no. 15) with a = 1650.0(5) pm, b = 945.6(3) pm, c = 1779.8(5) pm, β = 108.81(2)° (200 K); 5 in P21/n (no. 14) with a = 939.4(5) pm, b = 1736.8(6) pm, c = 1943.3(7) pm, β = 98.17(4)° (200 K). All compounds contain Z = 4 molecules in the unit cell.The 1H, 31P and 7Li NMR spectra of 2-6 are discussed.
    Notes: Es wird über die Verbindungen (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA) · [η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 und Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 berichtet. Letztere bilden sich durch Umsetzung der entsprechenden silylierten Triphosphane mit nBuLi: 2 und 3 aus (tBu2P)2P—SiMe3 1, 4 aus (iPr2P)2P—SiMe3, 5 aus (Et2N)2—P · (SiMe3)—PtBu2, 6 aus tBu2P—P(SiMe3)—PiPr2.1 kristallisiert orthorhombisch in P212121 (Nr. 19) mit a = 910,87(7) pm, b = 1132,5(1) pm, c = 2373,5(2) pm (bei 90 K bestimmt). Die Strukturbestimmung von 2 erfolgte bei 293 K und 200 K. 2 kristallisiert monoklin in P21/n (Nr. 14) mit a = 1069,7(3) pm, b = 1802,5(3) pm, c = 1604,0(7) pm, β = 98,11(2)° (200 K), 3 ebenfalls in P21/n (Nr. 14) mit a = 904,3(2) pm, b = 1936,4(5) pm, c = 1653,2(3) pm, β = 94,52(1)° (200 K). 4 kristallisiert monoklin in C2/c (Nr. 15) mit a = 1650,0(5) pm, b = 945,6(3) pm, c = 1779,8(5) pm, β = 108,81(2)° (200K), 5 in P21/n (Nr. 14) mit a = 939,4(5) pm, b = 1736,8(6) pm, c = 1943,3(7) pm, β = 98,17(4)° (200 K). Alle fünf Verbindungen enthalten jeweils vier Formeleinheiten in der Elementarzelle.Es wird über die Untersuchung der 1H-, 31P- und 7Li-NMR-Spektren der Verbindungen 2-6 berichtet.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220920
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