HRID653805

反应详情

EQUATION

反应方程式

HRID 653805 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 400 ml of toluene are dissolved 24.0 g of 2-amino-5-chlorothiophenol and 31.2 g of (4-methoxyphenyl)glycidic acid methyl ester, and the solution is refluxed under nitrogen atmosphere for 2 hours. To the reaction mixture are added 1.43 g of p-toluenesulfonic acid hydrate and 350 ml of xylene and the mixture is refluxed for 2 hours and simultaneously 350 ml of the solvent is distilled. After cooling, precipitated crystals are collected by filtration to give 19.8 g of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one.

WORKUP

后处理

  1. temperaturethe solution is refluxed under nitrogen atmosphere for 2 hours
  2. temperaturethe mixture is refluxed for 2 hours
  3. distillationsimultaneously 350 ml of the solvent is distilled
  4. temperatureAfter cooling
  5. customprecipitated crystals
  6. filtrationare collected by filtration