HRID23906
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
A mixture of 22 mmol of diethyl 2-(2,4,6-trifluorophenyl)malonate, 24 mmol of triethylamine and 22 mmol of 3-amino-1,2,4-triazole was heated with stirring at 180° C. for 6 hours. The reaction mixture was then cooled to 50° C., admixed with a solution of 2.2 g of sodium hydroxide in 25 ml of water and stirred for 30 minutes. The aqueous phase was washed with ether and then acidified with conc. hydrochloric acid. The precipitated colorless solid was filtered off, washed with water and diisopropyl ether and dried. The yield of the title compound was 85% (m.p.: 200-201° C.).
WORKUP
后处理
- temperaturewas heated
- temperatureThe reaction mixture was then cooled to 50° C.
- stirringstirred for 30 minutes
- washThe aqueous phase was washed with ether
- filtrationThe precipitated colorless solid was filtered off
- washwashed with water and diisopropyl ether
- customdried