反应详情

温度

70 °C

MeONa (2.27 g, 42 mmol) was added to a sol. of compounds D5 (22.6 g, 42 mmol) in MeOH (200 mL). The mixture was stirred at 70° C. for 6 h, and MeONa (2.27 g, 42 mmol) was added again. The mixture was stirred at 70° C. for 2 days, and was allowed to cool to rt. EtOAc was added, and the resulting mixture was washed with aq. 1M HCl and brine. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (MeOH/CH2Cl2 5:95→10:90) yielded the title compound (10.7 g, 47%). LC-MS: tR=1.19 min, ES+=538.39.

1. stirringThe mixture was stirred at 70° C. for 2 days
2. temperatureto cool to rt
3. washthe resulting mixture was washed with aq. 1M HCl and brine
4. dry with materiallayer was dried over MgSO4
5. filtrationfiltered
6. customthe solvents were removed under reduced pressure
7. customPurification of the crude by FC (MeOH/CH2Cl2 5:95→10:90)