公开(公告)号：US20060229469A1

公开(公告)日：2006-10-12

申请号：US10565542

申请日：2004-07-29

申请人： Oliver Huttenloch ,  Matthias Maase ,  Toni Flajs ,  Jurgen Werner

发明人： Oliver Huttenloch ,  Matthias Maase ,  Toni Flajs ,  Jurgen Werner

IPC分类号： C07F9/02

CPC分类号： C07F9/5036 ,  C07F9/5337

摘要： A process for the preparation of acylphosphines formula (1) wherein m is 1 or 2; R1, R2, and R3 are organic residues derived from aliphatic or aromatic hydrocarbons; by (1) reacting organic phosphorus halides of formula (II) wherein Y is Br or Cl,with an alkali metal in a solvent in the presence of an activator, wherein the alkali metal is present in the form of a dispersion of alkali metal particles having a mean particle size of ≦500 μm in the solvent, (2) subsequent reaction with acid halides of formula (III) which process is carried out without isolation of the intermediates. Preferably, R1, R2 and R3 are independently from each other phenyl, naphthyl and bi-phenyl, being unsubstituted or substituted by one to five halogen, C1-C8 alky and/or C1-C8 alkoxy. Most preferably, R1 and R3 are phenyl and R2 is 2,4,6-trimethylphenyl. The alkali metal is preferably sodium, the activator is preferably chlorobenzene and/or n-butanol.

摘要翻译： 制备其中m为1或2的式（1）的酰基膦的方法; R 1，R 2，R 3和R 3是衍生自脂族或芳族烃的有机残基; 通过（1）使其中Y为Br或Cl的式（II）的有机磷卤化物与碱金属在溶剂中在活化剂存在下反应，其中碱金属以碱金属颗粒分散体的形式存在 在溶剂中具有<=500μm的平均粒度，（2）随后与式（III）的酰卤反应，该方法在不分离中间体的情况下进行。 优选地，R 1，R 2和R 3 3彼此独立地为苯基，萘基和双 - 苯基，未被取代或被一个 至5个卤素，C 1 -C 8烷基和/或C 1 -C 8烷氧基。 最优选地，R 1和R 3是苯基，R 2是2,4,6-三甲基苯基。 碱金属优选为钠，活化剂优选为氯苯和/或正丁醇。

公开(公告)号：US20080146850A1

公开(公告)日：2008-06-19

申请号：US11815460

申请日：2006-02-09

申请人： Kathrin Wissel ,  Matthias Maase ,  Oliver Huttenloch ,  Toni Flajs ,  Melanie Kuhl

发明人： Kathrin Wissel ,  Matthias Maase ,  Oliver Huttenloch ,  Toni Flajs ,  Melanie Kuhl

IPC分类号： C07F9/50

CPC分类号： C07F9/5081 ,  C07F9/5068

摘要： Method for producing tertiary phosphines by reacting a compound of the general formula (I) in which A is R1 or L2, B is R2 or L3, the R1 and R2 radicals are each independently an organic radical having in each case from 1 to 30 carbon atoms, where the R1 and R2 radicals may also be joined together; and the leaving groups L1 to L3 are each independently halogen, alkyloxy having from 1 to 10 carbon atoms or aryloxy having from 6 to 10 carbon atoms (a) with an alkali metal in an organic aprotic solvent and (b) a compound of the general formula (II) L4-R3   (II) in which the R3 radical is an organic radical having in each case from 1 to 30 carbon atoms; and the leaving group L4 is halogen, alkyloxy having from 1 to 10 carbon atoms or aryloxy having from 6 to 10 carbon atoms, in which the resulting reaction mixture is hydrolyzed with an aqueous base which has a pH of ≧10 and the organic phase is removed from the aqueous phase.

摘要翻译： 通过使其中A为R 1或L 2的通式（I）的化合物与B 2反应生成叔膦的方法，B为R 2 O / >或L 3，R 1和R 2基团各自独立地为在每种情况下具有1至30个碳原子的有机基团， 其中R 1和R 2基团也可以连接在一起; 和离去基团L 1至L 3各自独立地为卤素，具有1至10个碳原子的烷氧基或具有6至10个碳原子的芳氧基（a）与 有机质子惰性溶剂中的碱金属和（b）通式（II）的化合物<？in-line-formula description =“In-line Formulas”end =“lead”→> L 4 （II）<？in-line-formula description =“In-line formula”end =“tail”？>其中R 3是基团 在每种情况下具有1至30个碳原子的有机基团; 并且离去基团L 4是卤素，具有1至10个碳原子的烷氧基或具有6至10个碳原子的芳氧基，其中所得反应混合物用具有pH值的碱水溶液水解 > 10，并且从水相中除去有机相。