反应详情

The sulfide 7A (900 mg, 1.63 mmol) was dissolved in chloroform (25 ml), cooled in an ice bath and m-chloroperbenzoic acid (300 mg, 57 to 80%, about 1 equiv) was added in small portions over 15 min. After 1 hr., the reaction was washed with 10% aqueous NaHSO3 solution, sat. aq. NaHCO3 solution (three times) and dried (Na2SO4). Removal of the solvent afforded 7B (740 mg, 90%) as a foam. Analytical HPLC retention time=1.99 min. (YMC Xterra S7 C18, 3.0×50 mm column, 10–90% aqueous methanol over 2 minutes containing 0.1% TFA, 5 mL/min, monitoring at 220 nm) and a LC/MS M++1=506.

1. temperaturecooled in an ice bath
2. wash, the reaction was washed with 10% aqueous NaHSO3 solution, sat. aq. NaHCO3 solution (three times)
3. dry with materialdried (Na2SO4)
4. customRemoval of the solvent