HRID1528536
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
To a solution of 3-trifluoromethylpyrazole (5.0 g, 36 mmol), triethylamine (7.0 mL, 50 mmol) in dichloromethane (40 mL) was added dimethylsulfamoyl chloride (5.5 mL, 51 mmol), and the reaction mixture was heated at reflux for 2 days. The resulting mixture was cooled to ambient temperature and filtered through a pad of silica gel using dichloromethane as eluent. The filtrate was then concentrated under reduced pressure to give an amber residue. The resulting residue was dissolved in diethyl ether. The ether solution was washed with water, dried (MgSO4), and concentrated under reduced pressure to give 8.71 g of the title compound.
WORKUP
后处理
- temperaturethe reaction mixture was heated
- temperatureat reflux for 2 days
- filtrationfiltered through a pad of silica gel
- concentrationThe filtrate was then concentrated under reduced pressure
- customto give an amber residue
- washThe ether solution was washed with water
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure