反应详情

温度

70 °C

INT 45 (500 mg, 1.43 mmol) was dissolved in THF (20 mL) and HBr (33% in AcOH, 15 eq) was added. The resulting mixture was stirred at 70° C. until completion of the reaction. The mixture was quenched with saturated aqueous sodium bicarbonate and extracted with EtOAc. The organic layer was washed with saturated aqueous sodium bicarbonate, water and brine, dried over sodium sulfate and concentrated. The crude product was purified by flash chromatography on silica gel (cyclohexane/EtOAc) to give INT 46.

1. customThe mixture was quenched with saturated aqueous sodium bicarbonate
2. extractionextracted with EtOAc
3. washThe organic layer was washed with saturated aqueous sodium bicarbonate, water and brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated
6. customThe crude product was purified by flash chromatography on silica gel (cyclohexane/EtOAc)
7. customto give INT 46