HRID362406

反应详情

EQUATION

反应方程式

HRID 362406 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-dibenz[b,e]azepine, 0.518 g of 4-[N-methyl-N-(2-methylbenzoyl)amino]benzoyl chloride and 0.182 g of triethylamine in 10 ml of tetrahydrofuran is stirred at room temperature for 2 hours. The solvent is removed, the residue diluted with water and extracted with dichloromethane. The extract is washed with 1N 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 solvent is removed
  2. additionthe residue diluted with water
  3. extractionextracted with dichloromethane
  4. washThe extract is washed with 1N HCl water, 1M NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. concentrationThe filtrate is concentrated
  7. temperaturechilled