反应详情

A mixture of sulfuric acid (3.9 ml), acetic acid (23.6 ml) and water (19.6 ml) was added to 3-bis(ethoxycarbonyl)acetyl-1-(4-fluorophenyl)-5-[4-(methylsulfonyl)phenyl]pyrazole. The mixture was refluxed for 5 hours and concentrated. The residue was dissolved in ethyl acetate, and the solution was washed with water, dried and concentrated. The residue was purified by column chromatography on silica gel (150 g) eluting with a mixture of chloroform and ethyl acetate (3:1) to give pale brown crystals of 3-acetyl-1-(4-fluorophenyl)-5-[4-(methylsulfonyl)phenyl]pyrazole (4.2 g).

1. temperatureThe mixture was refluxed for 5 hours
2. concentrationconcentrated
3. dissolutionThe residue was dissolved in ethyl acetate
4. washthe solution was washed with water
5. customdried
6. concentrationconcentrated
7. customThe residue was purified by column chromatography on silica gel (150 g)
8. washeluting with a mixture of chloroform and ethyl acetate (3:1)