反应详情

温度

66 °C

Compound 25 (1.0 equiv.) was dissolved in CH3OH (30 mL) with a magnetic stirrer at RT, and 35% H2O2 (3.0 equiv.) was added slowly to this solution. This reaction mixture was heated in an oil bath at 66° C. and monitored using TLC. The reaction was quenched with MnO2 at RT. The mixture was filtered and the residue was washed with ethyl acetate (3×5 mL). The liquid layer was concentrated under reduced pressure and the oily residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether) to provide a yellow solid; 44.3% yield;

1. customThe reaction was quenched with MnO2 at RT
2. filtrationThe mixture was filtered
3. washthe residue was washed with ethyl acetate (3×5 mL)
4. concentrationThe liquid layer was concentrated under reduced pressure
5. customthe oily residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether)
6. customto provide a yellow solid