HRID1589979

反应详情

EQUATION

反应方程式

HRID 1589979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

36.0 g (0.227 mol) of 2-acetyl-3-keto-4-methyl-4,5-dihydrothiophene are initially introduced into 260 ml of methylene chloride 21.9 ml of sulphuryl chloride in 260 ml of methylene chloride are then added dropwise at 0° C. While the sulphuryl chloride/methylene chloride mixture is added dropwise, a stream of nitrogen is passed into the solution to expel the HCl gas which is formed. When the addition is complete, stirring is continued for 30 minutes at 10°-15° C. The mixture is then introduced into 600 ml of water, and the organic phase is extracted with a 5% strength NaHCO3 solution, dried and concentrated in vacuo.

WORKUP

后处理

  1. additionare then added dropwise at 0° C
  2. customis formed
  3. additionWhen the addition
  4. extractionthe organic phase is extracted with a 5% strength NaHCO3 solution
  5. customdried
  6. concentrationconcentrated in vacuo