HRID414090

反应详情

EQUATION

反应方程式

HRID 414090 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10,1 g of 5-amino-1-(o-chlorobenzyl)-1H-triazole-4-carboxamide are added, portionwise with stirring, to a mixture of 30,7 g of acetanhydride and 0,1 ml of sulphuric acid and heated to 60° . Stirring is continued for additional 30 minutes at 60° to 70° , the reaction mixture is poored into 250 ml of ethanol, heated to reflux for 30 minutes and evaporated in vacuo to dryness. The residue is triturated with 250 ml of ethyl acetate, the crystalline precipitate is collected and re-crystallised from ethyl acetate yielding 5-acetylamino-1-(o-chlorobenzyl)-1H-1,2,3-triazole-4-carboxamide of m.p. 181°-183°.

WORKUP

后处理

  1. temperatureheated to 60°
  2. temperatureheated
  3. temperatureto reflux for 30 minutes
  4. customevaporated in vacuo to dryness
  5. customThe residue is triturated with 250 ml of ethyl acetate
  6. customthe crystalline precipitate is collected
  7. customre-crystallised from ethyl acetate