HRID372369

反应详情

EQUATION

反应方程式

HRID 372369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5.5 g hydrogen fluoride in toluene cooled to -65° C was added dropwise with stirring 15.0 ml of methylisocyanate over a period of 20 minutes after stirring for 1.5 hr preshly prepared 4-t-butylphenylthiosulfenyl chloride (prepared from 36.2 g 4-t-butylthiophenol and 31.0 g sulfur dichloride in 800 ml ethyl ether) was added at -10° to 0° C over a period of 0.5 hr. After stirring overnight at ambient temperature, the salt was removed by filtration and the filtrate distilled. b.p. 122°-127° C/0.2 Torr.

WORKUP

后处理

  1. additionwas added dropwise
  2. additionwas added at -10° to 0° C over a period of 0.5 hr
  3. customthe salt was removed by filtration
  4. distillationthe filtrate distilled