반응 #1914812

반응 방정식

2-hydrazinopyridine

3-ethoxyacrylonitrile

2-Hydrazinopyridine

→

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

용매

pentanol

반응 조건

후처리

1. 1
   온도to reflux for 5 h
2. 2
   온도to reflux for 4 h
3. 3
   농축the mixture is concentrated under reduced pressure until the excess hydrazinopyridine
4. 4
   기타has precipitated
5. 5
   기타The filtrate was purified by column chromatography

실험 절차

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%).

출처