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    Process for Preparing Acylphosphanes and Derivatives Thereof
    4.
    发明申请
    Process for Preparing Acylphosphanes and Derivatives Thereof 有权

    公开(公告)号：US20080004464A1

    公开(公告)日：2008-01-03

    申请号：US11667780

    申请日：2005-11-14

    申请人： Peter Murer ,  Jean-Pierre Wolf ,  Stephan Burkhardt ,  Hansjorg Grutzmacher ,  Daniel Stein ,  Kurt Dietliker

    发明人： Peter Murer ,  Jean-Pierre Wolf ,  Stephan Burkhardt ,  Hansjorg Grutzmacher ,  Daniel Stein ,  Kurt Dietliker

    IPC分类号： C07F9/50 ,  C07C69/66

    CPC分类号： G03F7/029 ,  C07F9/5036 ,  C07F9/5337 ,  C07F9/5537 ,  C07F9/65515 ,  C07F9/6552

    摘要： The invention relates to a process for the preparation of (bis)acylphosphanes of formula I, wherein n and m are each independently of the other 1 or 2; R1 if n=1, is e.g. unsubstituted or substituted C1-C18alkyl or C2-C18alkenyl, or phenyl, R1 if n=2, is e.g. a divalent radical of the monovalent radical defined above; R2 is e.g. C1-C18alkyl, C3-C12cycloalkyl, C2-C18alkenyl, mesityl, phenyl, naphthyl; R3 is one of the radicals defined under R1; the process comprises the steps a) contacting e.g. elemental phosphorous [P]∞, P(Hal)3 with a reducing metal optionally in the presence of a catalyst or an activator in a solvent to obtain metal phosphides Me3P or Me′3P2, wherein Me is an alkali metal and Me′ is an earth alkali metal or to obtain metal polyphosphides b) optionally adding a proton source, optionally in the presence of a catalyst or an activator to obtain metal dihydrogen phosphides MePH2; c) subsequent acylation reaction with m acid halides of formula III or m carboxylic acid esters of formula IV or, in case that in formula I m=1, with one carboxylic ester of formula IV followed by one acid halide of formula III or vice versa, wherein R is the residue of an alcohol and R2 is as defined above; d) alkylation reaction subsequent reaction with an electrophilic agent R1Hal or other electrophilic agents to obtain the compounds of formula I. An oxidation step may follow to obtain mono- and bisacylphosphane oxides or mono- and bisacylphosphane sulfides, which are used as photoinitiators.