HRID1033482

反应详情

EQUATION

反应方程式

HRID 1033482 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 8-chloro-2,3-dihydro-3-hydroxy-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one (36.0 g), acetic anhydride (50 ml), dimethylsulfoxide (100 ml), pyridine (3 ml) and toluene (100 ml) is stirred at room temperature for 3 days. Water is added to the mixture, and the mixture is extracted with ethyl acetate, and the extract is washed with water, and dried. The resultant is evaporated to remove the solvent, and diethyl ether is added to the residue. The precipitated crystal is collected by filtration to give 3-acetoxy-8-chloro-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one (24.5 g).

WORKUP

后处理

  1. extractionthe mixture is extracted with ethyl acetate
  2. washthe extract is washed with water
  3. customdried
  4. customThe resultant is evaporated
  5. customto remove the solvent, and diethyl ether
  6. additionis added to the residue
  7. filtrationThe precipitated crystal is collected by filtration