反应详情

温度

60 °C

To a solution of Intermediate 113d (263 mg, 0.36 mmol) in MeOH (2.5 mL) was added pyridinium p-toluenesulfonate (179 mg, 0.71 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 3-10% MeOH in DCM, to give the title compound (163 mg, 70%). LCMS (Method 4): Rt 3.00 min, m/z 653 [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