HRID1980529

反应详情

EQUATION

反应方程式

HRID 1980529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 25.1 ml (36.8 g, 0.200 mol) of chloromethyltrichlorosilane in 400 ml dry tetrahydrofuran was cooled to -78° under nitrogen and stirred vigorously while 48.0 ml (0.100 mol) of 2.1 molar phenyllithium was slowly dripped in over 1 hour. After stirring another 30 minutes at -78° the solution was allowed to warm to room temperature and evaporated to about 200 ml. Addition of 500 ml ether, filtration to remove precipitated lithium chloride, and evaporation of the filtrate left 25.0 g of liquid. Distillation gave 6.5 g (29%) of the title compound as a colorless liquid: bp 62°-82° (0.15 mm); nmr (CDCl3): δ3.3 (s, 2) and 7.1-7.9 (m, 5).

WORKUP

后处理

  1. customwas slowly dripped in over 1 hour
  2. customevaporated to about 200 ml
  3. additionAddition of 500 ml ether, filtration
  4. customto remove
  5. customprecipitated
  6. customlithium chloride, and evaporation of the filtrate
  7. waitleft 25.0 g of liquid
  8. distillationDistillation