反应详情

A solution of sulfide 3 (8.41 g, 44 mmol) in CH2Cl2 (100 ml) was cooled in an ice bath. mCPBA (84% purity, 27.1 g, 3 equiv.) was added portion wise and the resulting solution was stirred at RT for 16 h. An aqueous 1 M NaHSO3 solution (20 ml) was added, and the resulting suspension was vigorously stirred at RT for 30 min. The white m-chlorobenzoic acid precipitate was filtrated over a celite pad. The organic layer was washed with a saturated aqueous NaHCO3 solution (3×20 ml), dried over MgSO4, filtrated then concentrated under reduced pressure. Purification by flash column chromatography (eluent: pet. ether/AcOEt 1:1 then 3:7 then pure AcOEt) afforded sulfone 5 as a colorless liquid (8.41 g, 86%).

1. stirringthe resulting suspension was vigorously stirred at RT for 30 min
2. filtrationThe white m-chlorobenzoic acid precipitate was filtrated over a celite pad
3. washThe organic layer was washed with a saturated aqueous NaHCO3 solution (3×20 ml)
4. dry with materialdried over MgSO4
5. filtrationfiltrated
6. concentrationthen concentrated under reduced pressure
7. customPurification by flash column chromatography (eluent