反応 #574428

反応方程式

Cyclopentylhydrazine hydrochloride

sodium methoxide

(1-Ethoxypropylidene)malononitrile

→

1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carbonitrile

収率 70.0%

溶媒

ethanol

反応条件

後処理

1. 1
   温度the mixture was refluxed for 21 hours
2. 2
   温度The reaction mixture was cooled
3. 3
   その他the solvent was removed in vacuo
4. 4
   workup.ADDITIONThe residue was treated with water (150 ml)
5. 5
   ろ過the obtained precipitate was collected by filtration
6. 6
   洗浄washed with water
7. 7
   その他dried in a vacuum oven for 24 hours

実験手順

Cyclopentylhydrazine hydrochloride (20.9 g, 0.1 moles), 97% sodium methoxide (5.6 g, 0.1 moles) and ethanol (100 ml) were combined and stirred at room temperature under argon for 2.5 hours. (1-Ethoxypropylidene)malononitrile was added to the reaction mixture and the mixture was refluxed for 21 hours. The reaction mixture was cooled and the solvent was removed in vacuo. The residue was treated with water (150 ml) and the obtained precipitate was collected by filtration, washed with water and dried in a vacuum oven for 24 hours to afford 14.2 g (70%) of 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carbonitrile as a brown powder, m.p. 171°-173° C.

出典