HRID362398

反应详情

EQUATION

反应方程式

HRID 362398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 0.362 g of 4-[(6,11-dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl]benzoyl chloride and 0.101 g of triethylamine in 5 ml of dichloromethane is added a solution of 0.129 g of 2-methylaniline in 3 ml of dichloromethane. The mixture is stirred 1.5 hr at room temperature and then washed with H2O 1N HCl, 1M NaHCO3, brine and dried (Na2SO4). The solvent is removed to give a solid. The solid is dissolved in dichloromethane and filtered through a thin pad of hydrous magnesium silicate with dichloromethane as eluent to give 0.025 g of crystals, m.p. 214°-216° C.

WORKUP

后处理

  1. washwashed with H2O 1N HCl, 1M NaHCO3, brine
  2. dry with materialdried (Na2SO4)
  3. customThe solvent is removed
  4. customto give a solid
  5. filtrationfiltered through a thin pad of hydrous magnesium silicate with dichloromethane as eluent