反应详情

To a solution of Intermediate 103d (100 mg, 0.13 mmol) in MeOH (2 mL) was added pyridinium p-toluenesulfonate (65 mg, 0.26 mmol) and the reaction mixture was heated to reflux temperature for 3 h. The volatiles were concentrated in vacuo and the resultant residue was partitioned between EtOAc and water. The aqueous phase was extracted with EtOAc (×3) and the combined organic layers were washed with brine, dried (MgSO4) and concentrated in vacuo to afford the title compound (97 mg, 99%). LCMS (Method 2): Rt 3.39 min, m/z 681 [MH+].

1. temperaturethe reaction mixture was heated
2. temperatureto reflux temperature for 3 h
3. concentrationThe volatiles were concentrated in vacuo
4. customthe resultant residue was partitioned between EtOAc and water
5. extractionThe aqueous phase was extracted with EtOAc (×3)
6. washthe combined organic layers were washed with brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo