反应 #1914812

反应方程式

2-hydrazinopyridine

3-ethoxyacrylonitrile

2-Hydrazinopyridine

→

2-pyridin-2-yl-2H-pyrazol-3-ylamine

溶剂

pentanol

反应条件

后处理

1. 1
   温度to reflux for 5 h
2. 2
   温度to reflux for 4 h
3. 3
   浓缩the mixture is concentrated under reduced pressure until the excess hydrazinopyridine
4. 4
   其他has precipitated
5. 5
   其他The filtrate was purified by column chromatography

实验过程

A solution of 2-hydrazinopyridine (38.9 g, 453 mmol) was slowly added to a solution of 3-ethoxyacrylonitrile (31.5 g, 324 mmol) in pentanol (155 ml). The reaction mixture was brought to reflux for 5 h. 2-Hydrazinopyridine (10.6 g, 97 mmol) was again added and the reaction was allowed to continue to reflux for 4 h. The progress of the reaction is observed by TLC and, when the reaction is complete, the mixture is concentrated under reduced pressure until the excess hydrazinopyridine has precipitated. The filtrate was purified by column chromatography to give 2-pyridin-2-yl-2H-pyrazol-3-ylamine in the form of a white solid (2.75 g, 5.3%).

来源