反应详情

温度

80 °C

To a stirred Compound 62(850 mg, 3.66 mmol) was added PBr3(9.90 g, 36.6 mmol) with ice-cooling. The reaction mixture was stirred at 80° C. for 6 h. The mixture was diluted with water with ice-cooling and extracted with CH2Cl2. The combined solution was washed with sat. NaHCO3 and brine, dried(MgSO4) and concentrated in vacuo to give crude product as a yellow oil. The crude product was purified by column chromatography on silica gel with hexane-ethyl acetate(50:1-40:1) to give Compound 63(727 mg, 93%) as a yellow oil.

1. temperaturecooling
2. temperaturecooling
3. extractionextracted with CH2Cl2
4. washThe combined solution was washed with sat. NaHCO3 and brine, dried(MgSO4)
5. concentrationconcentrated in vacuo
6. customto give crude product as a yellow oil
7. customThe crude product was purified by column chromatography on silica gel with hexane-ethyl acetate(50:1-40:1)