HRID3564

反应详情

EQUATION

反应方程式

HRID 3564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.40 g of 10,11-dihydro-10-(3-methyl-4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.40 g of 2,4-dichlorobenzoyl chloride and 0.75 g of diisopropylethylamine in 50 ml of dichloromethane is stirred at room temperature for 16 hours. The mixture is washed with water, dried (MgSO4) and the solution passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated and hexane added to give crystals. Recrystallization from dichloromethane-hexane gives 0.52 g of crystals, m.p. 213°-215° C.

WORKUP

后处理

  1. washThe mixture is washed with water
  2. dry with materialdried (MgSO4)
  3. concentrationThe filtrate is concentrated
  4. additionhexane added
  5. customto give crystals
  6. customRecrystallization from dichloromethane-hexane