HRID1079338

反应详情

EQUATION

反应方程式

HRID 1079338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethanesulphonyl chloride (3.8 g) in dichloromethane (50 ml) was added dropwise at room temperature to a stirred solution of 2,3,4,5-tetrahydro-1,4-benzothiazepine (4.29 g, prepared as described in the first paragraph of Example 6 above) in dichloromethane (100 ml). The reaction mixture was stirred at room temperature for one hour, washed with water, dried and the solvent was removed by evaporation. Purification of the residue by flash chromatography using trichloromethane as eluent gave 4-ethylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from hexane. Yield 4.25 g (m.p. 78°-80° C.).

WORKUP

后处理

  1. customprepared
  2. washwashed with water
  3. customdried
  4. customthe solvent was removed by evaporation
  5. customPurification of the residue by flash chromatography