反应详情

To a solution of 29 mg of 20-methyl-1α,3β-bis(methoxycarbonyloxy)-21-phenylsulfinylpregna-5,7-diene in 1 ml of methanol was added 0.5 ml of a 30% aqueous solution of hydrogen peroxide and the mixture was stirred at ambient temperature for 6 hours. The reaction mixture was diluted with water and the methanol was distilled off under reduced pressure. The residue was extracted with methylene chloride, the extract was washed with an aqueous solution of sodium thiosulfate, water and an aqueous solution of sodium chloride, dried over sodium sulfate and concentrated. The residue was purified by silica gel column chromatography to give 13 mg of 20-methyl-1α,3β-bis(methoxycarbonyloxy)-21-phenylsulfonylpregna-5,7-diene, whose 1H NMR spectrum was identical with that obtained in Example 5.

1. distillationthe methanol was distilled off under reduced pressure
2. extractionThe residue was extracted with methylene chloride
3. washthe extract was washed with an aqueous solution of sodium thiosulfate, water
4. dry with materialan aqueous solution of sodium chloride, dried over sodium sulfate
5. concentrationconcentrated
6. customThe residue was purified by silica gel column chromatography