HRID345152

反应详情

EQUATION

反应方程式

HRID 345152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

In 30 ml of dimethylformamide are dissolved 0.9 g of 3-amino-2-(p-chlorophenyl)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine- 5-acetamide and 1.2 g of succinimido 2-indolecarboxylate, and the solution is stirred at 65° C. for 13 hours. The reaction mixture is concentrated under reduced pressure and a saturated aqueous solution of sodium hydrogencarbonate and ethyl acetate are added to the residue. The mixture is stirred for a while. The resulting crystals are collected by filtration, and the crystals are recrystallized from a mixed solvent of chloroform and methanol to give 0.8 g of 2-(p-chlorophenyl)-3-(2-indolecarboxamido)-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetamide, m.p. 275°-290° C. (decomposition).

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. additiona saturated aqueous solution of sodium hydrogencarbonate and ethyl acetate are added to the residue
  3. stirringThe mixture is stirred for a while
  4. filtrationThe resulting crystals are collected by filtration
  5. customthe crystals are recrystallized from a mixed solvent of chloroform and methanol