反应详情

To a solution of 7-(5-bromo-2-thienyl)-4-tert-butoxycarbonylperhydro-1,4-thiazepine (73.8 g) in methanol (500 ml) was added an aqueous solution (500 ml) of OXONE (2KHSO5.KHSO4.K2SO4) (156 g) under ice-cooling. After being stirred for 4 hours, the reaction mixture was concentrated in vacuo to remove methanol. The residue was extracted with ethyl acetate (1000 ml) and the extract was washed successively with a saturated aqueous solution of sodium bicarbonate and brine, dried over magnesium sulfate, and concentrated in vacuo. The residue was washed with hexane to afford 7-(5-bromo-2-thienyl)-4-tert-butoxycarbonylperhydro-1,4-thiazepine 1,1-dioxide (64.6 g) as a solid.

1. temperatureK2SO4) (156 g) under ice-cooling
2. concentrationthe reaction mixture was concentrated in vacuo
3. customto remove methanol
4. extractionThe residue was extracted with ethyl acetate (1000 ml)
5. washthe extract was washed successively with a saturated aqueous solution of sodium bicarbonate and brine
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated in vacuo
8. washThe residue was washed with hexane