反应详情

温度

80 °C

A mixture of 2'-(2,4-difluorophenoxy)-4'-formylmethanesulfonanilide (2.3 g) and triphenylphosphoranylideneacetone (2.3 g) in dimethylsulfoxide (10 ml) was stirred for 13 hours at 80° C. After cooling of the mixture, ethyl acetate was added, and the resulting mixture was washed with water, then dried. The ethyl acetate layer was evaporated to dryness and the residue was purified by column chromatography on silica gel (80 g) eluting with a mixture of chloroform and methanol (200:1) and further recrystallized from ethanol to give pale yellow needles of 2'-(2,4-difluorophenoxy)-4'-(3-oxo-1-butenyl)methanesulfonanilide (1.0 g).

1. additionwas added
2. washthe resulting mixture was washed with water
3. customdried
4. customThe ethyl acetate layer was evaporated to dryness
5. customthe residue was purified by column chromatography on silica gel (80 g)
6. washeluting with a mixture of chloroform and methanol (200:1)
7. customfurther recrystallized from ethanol