HRID1164122

反应详情

EQUATION

反应方程式

HRID 1164122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 2-cyano-2-[2-methoxy-3-(o-tolylthio)phenyl]acetate (4 g) in dimethylformamide (5 ml) was added dropwise to a solution of sodium hydride (purity 65%, 450 mg) in dimethylformamide (20 ml) in 10 minutes at temperature below 10° C. with stirring. After stirring the mixture at the same temperature for 10 minutes, n-hexyl bromide (3.85 g) was added to the mixture and stirred at 50° C. for an hour. After evaporation, water was added to the residue, and the mixture was extracted with diethyl ether. The extract was washed with water, dried and evaporated under reduced pressure to give oily ethyl 2-cyano-2-[2-methoxy-3-(o-tolylthio)phenyl]octanoate (5 g).

WORKUP

后处理

  1. stirringAfter stirring the mixture at the same temperature for 10 minutes
  2. stirringstirred at 50° C. for an hour
  3. customAfter evaporation, water
  4. additionwas added to the residue
  5. extractionthe mixture was extracted with diethyl ether
  6. washThe extract was washed with water
  7. customdried
  8. customevaporated under reduced pressure