反应详情

温度

45 °C

A solution of Intermediate 74h (0.34 g, 0.37 mmol) in MeOH (3.7 mL) was treated with pyridinium p-toluenesulfonate (0.28 g, 1.1 mmol) and the mixture was stirred at 45° C. for 24 h. The mixture was evaporated in vacuo and the residue was partitioned between DCM and a saturated aqueous sodium bicarbonate solution. The aqueous layer was then extracted with DCM (2×). The combined organic layers were washed with water, a saturated aqueous sodium bicarbonate solution and brine, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by FCC, using 0-8% MeOH in DCM, to give the title compound as a golden glass (142 mg, 46%). LCMS (Method 3): Rt 4.81 min, m/z 839.6 [MH+].

1. customThe mixture was evaporated in vacuo
2. customthe residue was partitioned between DCM
3. extractionThe aqueous layer was then extracted with DCM (2×)
4. washThe combined organic layers were washed with water
5. dry with materiala saturated aqueous sodium bicarbonate solution and brine, dried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe residue was purified by FCC