反应详情

To a stirred solution of 6-(3-bromo-2-hydroxypropoxy)-3,4-dihydroquinolin-2(1H)-one (0.2 g, 0.666 mmol) in DCM was added 4 Å molecular sieves powder (0.2 g) and pyridinium chlorochromate (0.287 g, 1.333 mmol). The reaction mixture was stirred at room temperature for 12 h. The reaction mixture was filtered through celite and washed with DCM (50 mL). The filtrate was concentrated and the crude product purified by flash chromatography on silica gel using 60% ethyl acetate in hexane to give 6-(3-bromo-2-oxopropoxy)-3,4-dihydroquinolin-2(1H)-one as an off white solid (0.15 g, 76%). LCMS: RT 0.67 min; LCMS (ES-API), m/z 298.0 (M+H).

1. filtrationThe reaction mixture was filtered through celite
2. washwashed with DCM (50 mL)
3. concentrationThe filtrate was concentrated
4. customthe crude product purified by flash chromatography on silica gel using 60% ethyl acetate in hexane