反应详情

To a stirred solution of Intermediate 2 (1.9 g, 6.33 mmol) in dichloromethane:acetonitrile (700 mL), m-CPBA (1.19 g, 6.96 mmol) was added and stirred at rt for 1 h. TLC showed completion of starting material and formation of a polar spot (TLC System: 10% methanol/chloroform, (Rf): 0.4). The reaction mixture was concentrated, diluted with dichloromethane (30 ml), and washed with saturated sodium bicarbonate solution (20 mL) and water (15 mL). The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The crude compound was purified by silica gel column chromatography with 1 to 1.5% methanol in chloroform as eluents to afford Intermediate 3 as colorless gummy solid. (1.4 g, 70%). MS m/z: 317.1 (ES+, M+H).

1. concentrationThe reaction mixture was concentrated
2. additiondiluted with dichloromethane (30 ml)
3. washwashed with saturated sodium bicarbonate solution (20 mL) and water (15 mL)
4. dry with materialThe organic layer was dried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe crude compound was purified by silica gel column chromatography with 1 to 1.5% methanol in chloroform as eluents