反应详情

To a solution of 52A (1.25 g, 4.98 mmol) in CCl4 (7 ML) was added NBS (0.89 g, 4.98 mmol) followed by catalytic AIBN and the mixture was heated to reflux for 4 hours. The reaction was cooled to room temperature, filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO2, 10% CH2Cl2/Hexane then 50% CH2Cl2/Hexane) to give 52B (0.90 g, 55%). HPLC Rt=2.85 min.

1. temperaturethe mixture was heated
2. temperatureto reflux for 4 hours
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was purified by flash chromatography (SiO2, 10% CH2Cl2/Hexane