HRID355908

反应详情

EQUATION

反应方程式

HRID 355908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.291 g of 6,11-dihydro-5H-di-benz[b,e]azepine, 0.518 g of 4-[N-methyl-N-(2-methyl-benzoyl)amino]benzoyl chloride and 0.182 g of triethylamine in 10 ml of tetrahydrofuran is stirred at room temperature for 2 hours. The solyent is removed, the residue diluted with water and extracted with dichloromethane. The extract is washed with 1 N HCl water, 1M NaHCO3, brine and dried (Na2SO4). The solution is passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated and chilled to give 0.52 g of crystals, m.p. 160°-170° C.

WORKUP

后处理

  1. customThe solyent is removed
  2. additionthe residue diluted with water
  3. extractionextracted with dichloromethane
  4. washThe extract is washed with 1 N HCl water, 1M NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. concentrationThe filtrate is concentrated
  7. temperaturechilled