反应详情

The compound (1.05 g) obtained in Step 2 was suspended in chloroform (50 ml), manganese dioxide (4.86 g) was added, with stirring at room temperature, and the mixture was stirred at the same temperature for 3 days. The reaction mixture was concentrated, tetrahydrofuran (150 ml) and activated carbon were added, and the mixture was heated under reflux. The insoluble material was filtered off when it was hot, and the insoluble material was washed with a heated mixed solvent (tetrahydrofuran:N,N-dimethylformamide:methanol=8:1:1). The filtrate was concentrated under reduced pressure, and the obtained crude crystals were suspended in diethyl ether, collected by filtration and dried to give the title compound (782 mg).

1. stirringthe mixture was stirred at the same temperature for 3 days
2. concentrationThe reaction mixture was concentrated
3. additiontetrahydrofuran (150 ml) and activated carbon were added
4. temperaturethe mixture was heated
5. temperatureunder reflux
6. filtrationThe insoluble material was filtered off when it
7. washthe insoluble material was washed with a heated
8. additionmixed solvent (tetrahydrofuran:N,N-dimethylformamide:methanol=8:1:1)
9. concentrationThe filtrate was concentrated under reduced pressure
10. customthe obtained crude crystals
11. filtrationcollected by filtration
12. customdried