HRID5579
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturecooling
- stirringthe mixture is stirred at room temperature overnight
- filtrationthe precipitated crystals are collected by filtration
- customdried