HRID1293149
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
- 50 °C
PROCEDURE
实验过程
A mixture of 3,5-dimethylpyrazole (100 mg), 3-chlorosulfonyl-1-dimethylcarbamoyl-1H-1,2,4-triazole (Example 54-a) (480 mg), anhydrous potassium carbonate (280 mg), and acetonitrile (1.5 ml) was heated and stirred for 2 hours on an oil bath at 50° C. The reaction solution was extracted with ethyl acetate-water. The organic layer was washed with saturated aqueous sodium chloride solution, and concentrated. The residue was subjected to a silica-gel column chromatography with 20 to 30% (20% 2-propanol/ethyl acetate)/hexane, and the title compound (210 mg) was obtained by crystallization in ethyl acetate-hexane.
WORKUP
后处理
- temperaturewas heated
- extractionThe reaction solution was extracted with ethyl acetate-water
- washThe organic layer was washed with saturated aqueous sodium chloride solution
- concentrationconcentrated