반응 #334220

반응 방정식

2-hydroxyethylhydrazine

ethoxymethylenemalononitrile

→

5-amino-4-cyano-1-(2-hydroxyethyl)pyrazole

수율 70.3%

용매

EtOH

EtOH

반응 조건

후처리

1. 1
   workup.ADDITIONwas added over a period of ten minutes
2. 2
   세척The last of this material was washed into the reaction flask with EtOH (50 ml.)
3. 3
   온도the mixture was heated
4. 4
   온도under reflux for 2.5 hours
5. 5
   기타The golden-brown crystals which formed
6. 6
   여과were collected by filtration
7. 7
   세척washed with ether
8. 8
   기타dried in vacuo at room temperature

실험 절차

A solution of 2-hydroxyethylhydrazine (38.9 g.) in EtOH (425 ml.) was heated to 50° while a solution of ethoxymethylenemalononitrile (52 g.) in warm EtOH (250 ml.) was added over a period of ten minutes. The last of this material was washed into the reaction flask with EtOH (50 ml.), and the mixture was heated under reflux for 2.5 hours. The resulting solution was allowed to cool to room temperature overnight. The golden-brown crystals which formed were collected by filtration, washed with ether, and dried in vacuo at room temperature to give 5-amino-4-cyano-1-(2-hydroxyethyl)pyrazole (45.57 g.): m.p. 158°-160 °.

출처