HRID247038

反应详情

EQUATION

反应方程式

HRID 247038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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 °.

WORKUP

后处理

  1. additionwas added over a period of ten minutes
  2. washThe last of this material was washed into the reaction flask with EtOH (50 ml.)
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for 2.5 hours
  5. customThe golden-brown crystals which formed
  6. filtrationwere collected by filtration
  7. washwashed with ether
  8. customdried in vacuo at room temperature