HRID638477
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 mixture of 250 ml of methylene chloride, 250 ml of water and 250 ml of 30% ammonia solution is slowly added a solution of 80.3 g of crude 2-difluoromethoxyphenylsulfonyl chloride in 50 ml of methylene chloride. After the exothermic reaction has subsided, the reaction mixture is refluxed for 2 hours. The organic phase is washed with water, dried over sodium sulfate, and evaporated to dryness. Recrystallisation from methanol yield 40.5 g of 2-difluoromethoxyphenylsulfonamide with a melting point of 128°-130° C.
WORKUP
后处理
- customAfter the exothermic reaction
- temperaturethe reaction mixture is refluxed for 2 hours
- washThe organic phase is washed with water
- dry with materialdried over sodium sulfate
- customevaporated to dryness
- customRecrystallisation from methanol yield 40.5 g of 2-difluoromethoxyphenylsulfonamide with a melting point of 128°-130° C.