HRID544516

反应详情

EQUATION

反应方程式

HRID 544516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 27.2 g (0.2 mole) of tetravinyl silane and 149.5 g (0.804 mole) diphenylphosphine was reacted in a quartz pressure tube at 200° C. with u.v. light initiation until most of the diphenyl phosphine was converted. The hot, molten reaction mixture was added to 720g of hot toluene with stirring. The tetraaduct product precipitated from the solution as a white crystalline solid. The mixture was allowed to coolto ambient temperature and then filtered with suction. After washing with toluene and drying in vacuo, 84 g (47.7%) of crude product was obtained. This was recrystallized from 1200 ml of xylene to obtain 69 g of the pure tetrakis-(diphenylphosphinoethyl) silane of mp. 198°-199° C.

WORKUP

后处理

  1. customwas reacted in a quartz pressure tube at 200° C. with u.v
  2. customThe tetraaduct product precipitated from the solution as a white crystalline solid
  3. customto coolto ambient temperature
  4. filtrationfiltered with suction
  5. washAfter washing with toluene
  6. customdrying in vacuo
  7. custom84 g (47.7%) of crude product was obtained
  8. customThis was recrystallized from 1200 ml of xylene