反应详情

K2CO3 (1.5 g, 11 mmol) was added to a solution of 52B (800 mg, 2.2 mmol) in MeOH/H2O (2:1, 9 mL) and the mixture was refluxed for 2 h. Volatiles were removed in vacuo and the remaining aqueous mixture was extracted with EtOAc. The combined organics were washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by flash chromatography (0% to 100% EtOAc in hexanes) to yield 52C (275 mg, 47%) as a clear oil. MS (ESI) m/z 267.1 (M+H)+.

1. temperaturethe mixture was refluxed for 2 h
2. customVolatiles were removed in vacuo
3. extractionthe remaining aqueous mixture was extracted with EtOAc
4. washThe combined organics were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by flash chromatography (0% to 100% EtOAc in hexanes)