反应详情

A mixture of 4'-amino-3'-(2,4-difluorophenylamino)acetophenone (1.7 g) and methanesulfonyl chloride (0.9 g) in pyridine (17 ml) was stirred for 4 hours at room temperature. Pyridine was evaporated and the residue was stirred with an aqueous solution of sodium hydroxide (5%) for 30 minutes. The solution was washed with toluene, acidified to pH 3 with hydrochloric acid, and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium bicarbonate, dried, and concentrated under reduced pressure. The syrupy residue (1.8 g) was crystallized from ethanol to give pale yellow crystals of 4'-acetyl-2'-(2,4-difluorophenylamino)methanesulfonanilide (1.3 g).

1. customPyridine was evaporated
2. stirringthe residue was stirred with an aqueous solution of sodium hydroxide (5%) for 30 minutes
3. washThe solution was washed with toluene
4. extractionextracted with ethyl acetate
5. washThe extract was washed with an aqueous solution of sodium bicarbonate
6. customdried
7. concentrationconcentrated under reduced pressure
8. customThe syrupy residue (1.8 g) was crystallized from ethanol