反応 #1914812

反応方程式

2-hydrazinopyridine

3-ethoxyacrylonitrile

2-Hydrazinopyridine

→

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

溶媒

pentanol

反応条件

後処理

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

実験手順

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%).

出典