HRID358183
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
PROCEDURE
实验过程
12 g (0.07 mol) of N-(2,2,2-trifluoroethyl)-N-methyl-hydroxyacetic acid amide and 4.5 g of potassium hydroxide powder were dispersed in 100 ml of acetonitrile at 0° C., and a solution of 12 g of 2-chloro-5-phenyl-1,3,4-thiadiazole in 50 ml of acetonitrile was added at 10° C. The mixture was stirred at 30° to 40° C. for 15 hours and concentrated, the concentrate was diluted with water and the mixture was filtered. The crystalline product was recrystallized from isopropanol. 12 g (63% of theory) of N-(2,2,2-trifluoroethyl)-N-methyl-5-phenyl-1,3,4-thiadiazol-2-yl-oxyacetic acid amide of melting point 123° C. were obtained.
WORKUP
后处理
- concentrationconcentrated
- additionthe concentrate was diluted with water
- filtrationthe mixture was filtered
- customThe crystalline product was recrystallized from isopropanol