HRID17831

反应详情

EQUATION

反应方程式

HRID 17831 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. additionwas added slowly
  2. temperatureAfter cooling to rt
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additionthe resulting residue treated with EtOH (6 ml) and water (6 ml)
  5. temperatureAfter cooling in an ice/water bath for 10 min
  6. filtrationthe resulting precipitate was collected by filtration