Reaktion #1914812

Reaktionsgleichung

2-hydrazinopyridine

3-ethoxyacrylonitrile

2-Hydrazinopyridine

→

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

Lösungsmittel

pentanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux for 5 h
2. 2
   Temperaturto reflux for 4 h
3. 3
   Einengenthe mixture is concentrated under reduced pressure until the excess hydrazinopyridine
4. 4
   Sonstigehas precipitated
5. 5
   SonstigeThe filtrate was purified by column chromatography

Vorschrift

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%).

Quelle