反応 #5675

反応方程式

5-dimethylamino-2,3,4,5-tetrahydro-1H-benzazepine

potassium carbonate

p-nitrobenzoyl chloride

→

5-dimethylamino-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine

収率 97.1%

溶媒

water

acetone

water

反応条件

後処理

1. 1
   温度cooling
2. 2
   workup.STIRRINGthe mixture is stirred at room temperature overnight
3. 3
   ろ過the precipitated crystals are collected by filtration
4. 4
   その他dried

実験手順

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.

出典