反应 #979942

反应方程式

tin dichloride dihydrate

N-(4-cyanophenyl)-4-amino-3-nitropyridine

ethanol

→

3-Amino-4-(4'-cyanophenyl)aminopyridine

溶剂

hydrochloric acid

water

反应条件

后处理

1. 1
   温度the resulting mixture was heated
2. 2
   温度to reflux for 10 minutes under nitrogen
3. 3
   温度The mixture was cooled in ice
4. 4
   过滤filtered
5. 5
   洗涤The creamy-coloured solid was washed with 2N aqueous sodium hydroxide and water
6. 6
   其他dried in a vacuum desiccator

实验过程

According to a modification of the method of Pharm. Helv. Acta, 1975, 50, 188., tin dichloride dihydrate (56.4 g, 250 mmol) was added to a suspension of N-(4-cyanophenyl)-4-amino-3-nitropyridine (12.0 g, 50 mmol) in 2N aqueous hydrochloric acid (35 ml), water (150 ml) and ethanol (75 ml) and the resulting mixture was heated to reflux for 10 minutes under nitrogen. The mixture was cooled in ice, poured into ice-cold 2N aqueous sodium hydroxide (400 ml) and filtered. The creamy-coloured solid was washed with 2N aqueous sodium hydroxide and water, and then dried in a vacuum desiccator. The product, 3-amino-4-(4'-cyanophenyl)aminopyridine, 9.31 g, gradually turns reddish brown on exposure to light and air.

来源