反应详情

温度

60 °C

To a solution of Intermediate 141a (214 mg, 0.28 mmol) in MeOH (3.0 mL) was added pyridinium p-toluenesulfonate (141 mg, 0.56 mmol) and the reaction mixture was heated at 60° C. for 3 h. The resultant mixture was poured into water and a saturated aqueous solution of NaHCO3 was added. The aqueous phase was extracted with EtOAc (×3) and the combined organic layers were washed with brine, dried (MgSO4) and concentrated in vacuo. The resultant residue was purified by FCC on silica, using a gradient of 0-10% MeOH in DCM, to give the title compound (132 mg, 69%). LCMS (Method 4): Rt 3.04 min, m/z 681 [MH+].

1. extractionThe aqueous phase was extracted with EtOAc (×3)
2. washthe combined organic layers were washed with brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe resultant residue was purified by FCC on silica