반응 #46109

반응 방정식

Hydrazine monohydrate

(1-Ethoxyethylidene)malononitrile

water

→

5-amino-3-methyl-1H-pyrazole-4-carbonitrile

수율 71.1%

용매

EtOH

반응 조건

후처리

1. 1
   workup.ADDITIONwas added slowly
2. 2
   온도After cooling to rt
3. 3
   농축The mixture was concentrated under reduced pressure
4. 4
   workup.ADDITIONthe resulting residue treated with EtOH (6 ml) and water (6 ml)
5. 5
   온도After cooling in an ice/water bath for 10 min
6. 6
   여과the resulting precipitate was collected by filtration

실험 절차

Hydrazine monohydrate (6.8 ml, 0.14 mol) was dissolved in EtOH (10 ml) and cooled to 0° C. (1-Ethoxyethylidene)malononitrile (10 g, 0.073 mol) was added slowly and the mixture was heated at 95° C. for 2 h. After cooling to rt, water (20 ml) was added and the mixture was allowed to stand at rt overnight. The mixture was concentrated under reduced pressure and the resulting residue treated with EtOH (6 ml) and water (6 ml). After cooling in an ice/water bath for 10 min, the resulting precipitate was collected by filtration to give 6.34 g of 5-amino-3-methyl-1H-pyrazole-4-carbonitrile.

출처