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  • 1
    ISSN: 0044-2313
    Keywords: Organophosphorus compounds, bicyclic hydrophosphorylation, intramolecular ; methylenebisphosphines ; 1,3-diphosphorinances ; 1,5-diphosphabicyclo[3.3.1]nonanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 1,5-Diphosphabicyclo [3.3.1]nonane1,5-Diphosphabicyclo[3.3.1]nonane 8 has been obtained by free-radical cyclization of CH2=CHCH2(H)PCH2P(H)CH2CH=CH2 6 and 1-allyl-1,3-diphosphorinane 7. For the synthesis of 6 and 7 the chlorophosphine Cl2PCH2PCl2 1 is used as a starting material, which can be converted into Me2N(Cl)PCH2P(Cl)NMe2 3 by reaction with (Me2N)2PCH2P(NMe2)2 2. Treatment of 3 with two equivalents of allyl lithium and cleavage of the PN bonds in CH2=CHCH2(Me2N)PCH2P(NMe2)CH2CH=CH2 4 with diluted HCl affords CH2=CHCH2(H)(O)PCH2P(O)(H)CH2CH=CH2 5. Phenylsilane is used for the first time as a reducing agent to obtain a secundary phosphine like 6 from the secundary phosphine oxide (5). Prolonged heating increases the yield of the byproduct 7 in the mixture of 6 and 7. Reactions of the trivalent phosphorus in 8 with CS2, CH3I, POCl3, NO, sulfur, and KSeCN, respectively, delivers the corresponding derivatives 9-17. The compounds decribed are characterized by 1H, 13C, 31P, 77Se n.m.r., i.r., and m.s. data.
    Notes: 1,5-Diphosphabicyclo[3.3.1]nonan 8 wird durch radikalische Cyclisierung von CH2=CHCH2(H)PCH2P(H)CH2CH=CH2 6 und 1-Allyl-1,3-diphosphorinan 7 erhalten. Ausgangsmaterial für die Synthese von 6 und 7 ist Cl2PCH2PCl2 1, das mit (Me2N)2PCH2P(NMe2)22 quantitativ zu Me2N(Cl)PCH2P(Cl)NMe2 3 reagiert. Die Umsetzung von 3 mit zwei Äquivalenten Allyllithium zu CH2=CHCH2(Me2N)PCH2P(NMe2)CH2CH=CH2 4 und Abspaltung der Me2N-Schutzgruppen mit verdünnter Salzsäure liefert CH2=CHCH2(H)(O)PCH2P(O)(H)CH2CH=CH2 5. Dessen Reduktion zu 6 gelingt mit C6H5SiH3. Daneben entsteht 7, das durch längeres Erhitzen angereichert werden kann. Reaktionen des dreibindigen Phosphors in 8 mit CS2, CH3I, POCl3, NO, Schwefel und KSeCN führen zu den Derivaten 9-17. Die Verbindungen werden durch 1H-, 13C-, 31P- und 77Se-NMR-sowie IR- und MS-Daten charakterisiert.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: I. r. and 31P n. m. r. spectroscopy ; bis(phosphane) sulphur dioxide nickel(0) complexes ; X-ray structure of Ni(PCy3)2(SO2) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulphur Dioxide as Ligand and Synthon. X. The Coordination Geometry of SO2 in Bis(phosphane)-Sulphur Dioxide-Nickel(0) Complexes. Structure of Ni(PCy3)2(SO2)The SO2 coordination geometry in Ni(PR3)2(SO2) complexes with steric parameters of the coligands Θ ≫ 141° was investigated by means of IR and 31P-NMR spectroscopy. The X-ray structure of Ni(PCy3)2(SO2) is described. The hitherto discussed n2-S.O-SO2 coordination mode for this type of complexes couldn't be confirmed.
    Notes: Zur Ermittlung der SO2-Koordinationsgeometrie in Ni(PR3)2(SO2)-Komplexen deren Coliganden Kegelöffnungswinkel von Θ ≫ 141° aufweisen, wurden die IR-und 31P-NMR-Spektroskopie herangezogen. Die Einkristallröntgenstrukturanalyse von Ni(PCy3)2(SO2) wird beschrieben. Eine für diesen Komplextyp bislang diskutierte n2-S.O-Koordination des Schwefeldioxids ließ sich nicht bestätigen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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