HRID1450013

反应详情

EQUATION

反应方程式

HRID 1450013 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

409.7 g (0.6 mol) of 2,2'-bis(diphenylphosphinylmethyl)-1,1'-binaphthyl are suspended in 1.5 1 of xylene and 715 ml (3.0 mol) of tri-n-butylamine in the absence of air and moisture, and 345.1 g (3.0 mol) of methyldichlorosilane are added dropwise with stirring. The mixture is then refluxed for 12 hours to give a clear solution. Xylene is distilled off at atmospheric pressure, and the mixture is allowed to cool with stirring. This results in the formation of 2,2'-bis(diphenylphosphinomethyl)-1,1'-binaphthyl as a colorless solid, which is filtered off under an inert gas and washed with 200 ml of degassed acetone. 378 g (97%) of colorless crystals of melting point 160° to 161° C. are obtained.

WORKUP

后处理

  1. additionare added dropwise
  2. temperatureThe mixture is then refluxed for 12 hours
  3. customto give a clear solution
  4. distillationXylene is distilled off at atmospheric pressure
  5. temperatureto cool
  6. stirringwith stirring