反应详情

Solid NaHCO3 (1.2 mol) and mCPBA (1 2 mmol, 77% purity) were added to a solution of ketone 1A (0.6 mmol) in DCM (5 mL) at 0° C. The reaction mixture was allowed to warm to rt and was maintained for 1 h. The reaction mixture was diluted with a saturated, aqueous solution of sodium bisulfate (10 mL) and was extracted with DCM (3×10 mL). The combined organic layers were dried (Na2SO4) and concentrated. The residue was purified by silica gel chromatography (10/90 to 30/70 EtOAc/hexane) to provide lactone 16A in 90% yield. Data: LC/MS (ESR) m/z 224 [M+1]+.

1. temperaturewas maintained for 1 h
2. extractionwas extracted with DCM (3×10 mL)
3. dry with materialThe combined organic layers were dried (Na2SO4)
4. concentrationconcentrated
5. customThe residue was purified by silica gel chromatography (10/90 to 30/70 EtOAc/hexane)