HRID5579

反应详情

EQUATION

反应方程式

HRID 5579 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5-dimethylamino-2,3,4,5-tetrahydro-1H-benzazepine (50 g) in a mixture of acetone (400 ml) and water (200 ml) is added potassium carbonate (38.8 g), and thereto is added p-nitrobenzoyl chloride (40 g) with stirring under ice-cooling, and the mixture is stirred at room temperature overnight. To the reaction mixture is added an appropriate amount of water, and the precipitated crystals are collected by filtration and dried to give 5-dimethylamino-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (71 g) as pale yellow powder, mp. 139°-142° C.

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture is stirred at room temperature overnight
  3. filtrationthe precipitated crystals are collected by filtration
  4. customdried