HRID610732

反应详情

EQUATION

反应方程式

HRID 610732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Hydrosilation of phenylacetylene with bis(dichlorosilyl)methane in the presence of Pd(PPh3)4. Into the same apparatus as described in Example 1 were added 1 g of bis(dichlorosilyl)methane, 0.101 g of Pd(PPh3)4, and 20 ml of dried benzene. The flask content was heated to reflux and 0.52 ml of phenylacetylene was added over a ten minute period. The flask content was refluxed, with stirring, for another hours and then the solvent removed at atmospheric pressure. The products were vacuum distilled at 67 Pa to give a mixture comprising 0.89 g of 1,1,3,3-tetrachloro-4-phenyl-1,3-disilacyclopent-4-ene (TCD-GC area 48.2%) and 3,3,5,5-tetrachloro-1,7-diphenyl-3,5-disilahepta-1,6-diene (TCD-GC area6%).

WORKUP

后处理

  1. temperatureThe flask content was heated
  2. temperatureto reflux
  3. temperatureThe flask content was refluxed
  4. customthe solvent removed at atmospheric pressure
  5. distillationdistilled at 67 Pa