HRID1247984

反应详情

EQUATION

反应方程式

HRID 1247984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.2 g of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(dimethylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, 1.16 g of 3,4-dinitrobenzoic acid and 0.76 g of dicyclohexylcarbodiimide are dissolved in 20 ml of methylene chloride, and the solution is stirred at room temperature overnight. After the reaction, the precipitates are collected by filtration. The filtrate is washed with water, dried and then evaporated to remove solvent. The residue is purified by silica gel chromatography (solvent, chloroform:methanol=100:3), whereby 0.8 g of (+)-cis-2-(4-methoxyphenyl)-3-(3,4-dinitrobenzoyloxy)-5-[2-(dimethylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one is obtained as an oil.

WORKUP

后处理

  1. customAfter the reaction
  2. filtrationthe precipitates are collected by filtration
  3. washThe filtrate is washed with water
  4. customdried
  5. customevaporated
  6. customto remove solvent
  7. customThe residue is purified by silica gel chromatography (solvent, chloroform:methanol=100:3)