HRID1283683

反应详情

EQUATION

反应方程式

HRID 1283683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 19.3 g. of methylene bromide and 3.7 g. of treithylamine in 100 ml. of dimethylformamide was added 10.0 g. of potassium p-chlorophenoxymethyldithiocarbamate in portions. After another 1 to 2 hours, the mixture was poured into water and partitioned into ethylene chloride. The dried ethylene chloride mixture was saturated with dry hydrogen chloride and the resulting salt collected by filtration. Hydrolysis of the salt in a chloroform-water mixture followed by separation, drying and concentration of the chloroform layer gave 3.5 g. of the dithietane as pale yellow crystals, m.p. 64.5°-66.0°C.

WORKUP

后处理

  1. additionTo a mixture of 19.3 g
  2. custompartitioned into ethylene chloride
  3. filtrationthe resulting salt collected by filtration
  4. customHydrolysis of the salt in a chloroform-water mixture
  5. customfollowed by separation
  6. customdrying
  7. customconcentration of the chloroform layer gave 3.5 g