反应详情

A mixture of 4-fluorobenzenesulfonyl chloride (III, Aldrich, 3.12 g), methylamine hydrochloride (1.17 g), triethylamine (4.8 ml) and THF (25 ml) are stirred at 20°-25° for five days. The mixture is then partitioned between dichloromethane, aqueous sodium bicarbonate, and saline. The organic phases are dried over magnesium sulfate and concentrated. The resulting solid is crystallized from dichloromethane/hexane and then recrystallized from methanol/dichloromethane to give N-methyl-4-fluorobenzenesulfonamide, NMR 2.67, 4.55, 7.21, 7.89 δ.

1. customThe mixture is then partitioned between dichloromethane, aqueous sodium bicarbonate, and saline
2. dry with materialThe organic phases are dried over magnesium sulfate
3. concentrationconcentrated
4. customThe resulting solid is crystallized from dichloromethane/hexane
5. customrecrystallized from methanol/dichloromethane