반응 #574428

반응 방정식

Cyclopentylhydrazine hydrochloride

sodium methoxide

(1-Ethoxypropylidene)malononitrile

→

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

수율 70.0%

용매

ethanol

반응 조건

후처리

1. 1
   온도the mixture was refluxed for 21 hours
2. 2
   온도The reaction mixture was cooled
3. 3
   기타the solvent was removed in vacuo
4. 4
   workup.ADDITIONThe residue was treated with water (150 ml)
5. 5
   여과the obtained precipitate was collected by filtration
6. 6
   세척washed with water
7. 7
   기타dried in a vacuum oven for 24 hours

실험 절차

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.

출처