HRID969741

反应详情

EQUATION

反应方程式

HRID 969741 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of 14 g (0.17 mol) of 3-amino-1,2,4-triazole, 34.3 g (0.17 mol) of diethyl 2-isopropylmalonate and 50 ml of tributylamine were stirred at 180° C. for 6 h. The reaction mixture was then cooled to 70° C., an aqueous solution of sodium hydroxide (21 g/200 ml of water) was added and the mixture was stirred for 30 min. The organic phase was separated and the aqueous phase was extracted with diethyl ether. The aqueous phase was then acidified using conc. hydrochloric acid and the resulting precipitate was collected by filtration. Drying gave 27 g (0.14 mol) of the title compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled to 70° C.
  2. stirringthe mixture was stirred for 30 min
  3. customThe organic phase was separated
  4. extractionthe aqueous phase was extracted with diethyl ether
  5. filtrationthe resulting precipitate was collected by filtration
  6. customDrying