反应详情

Sodium borohydride (0.2 g) was added portionwise to a solution of 4'-acetyl-2'-(2,4-difluorophenylthio)methanesulfonanilide (1.55 g) in methanol (30 ml) at 15° C. The mixture was stirred overnight at room temperature, treated with acetic acid, and concentrated under reduced pressure. The residue was dissolved in ethyl acetate, washed with an aqueous solution of sodium bicarbonate, dried, and concentrated. The residual oil (1.6 g) was purified by column chromatography on silica gel (50 g) eluting with a mixture of toluene and ethyl acetate (4:1). The purified product was recrystallized from a mixture of ethanol and water (2:1) to give crystals of 2'-(2,4-difluorophenylthio)-4'-(1-hydroxyethyl)methanesulfonanilide (1.03 g).

1. concentrationconcentrated under reduced pressure
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with an aqueous solution of sodium bicarbonate
4. customdried
5. concentrationconcentrated
6. customThe residual oil (1.6 g) was purified by column chromatography on silica gel (50 g)
7. washeluting with a mixture of toluene and ethyl acetate (4:1)
8. customThe purified product was recrystallized from a mixture of ethanol and water (2:1)