HRID1636803

反应详情

EQUATION

反应方程式

HRID 1636803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,2'-(5-hydroxymethyl-1,3-phenylene)di-(2-methylpropiononitrile), (3.8 g) and pyridine (1.58 g) in dichloromethane (10 ml) was stirred, and cooled in an ice bath, while thionyl chloride (3 g) was added over 10 minutes. The solution was kept at room temperature for 2 h and then heated under reflux for 1 h and evaporated to dryness under reduced pressure The residue was partitioned between water and ethyl acetate and the organic phase was separated, dried and evaporated to dryness under reduced pressure to give 2,2'-(5-chloromethyl-1,3-phenylene)di(2-methylpropiononitrile), which was used without further purification.

WORKUP

后处理

  1. additionwas added over 10 minutes
  2. temperatureheated
  3. temperatureunder reflux for 1 h
  4. customevaporated to dryness under reduced pressure The residue
  5. customwas partitioned between water and ethyl acetate
  6. customthe organic phase was separated
  7. customdried
  8. customevaporated to dryness under reduced pressure