反应详情

Carbon tetrachloride (CCl4, 300 mL) and the product from Example 1 (50.6 g, 0.26 mol) were placed in a 1-L flask equipped with a N2 inlet The solution was stirred until all solid dissolved. N-bromosuccinimide (NBS, 46.8 g, 0.26 mol) was then added to the reaction flask, followed by 2,2'-azobisisobutyronitrile (AIBN, 0.02 g). The reaction was heated to reflux for 7 h with a 500 watt reflector spot lamp. After cooling the reaction to room temperature, it was filtered and all solvent was removed under reduced pressure. Flash chromatography (15/85 ethyl acetate (EtOAc)/Hex) provided 24.89 g (37%) of title product.

1. customequipped with a N2 inlet The solution
2. dissolutiondissolved
3. temperatureThe reaction was heated
4. temperatureto reflux for 7 h with a 500 watt reflector spot lamp
5. temperatureAfter cooling
6. customthe reaction to room temperature
7. filtrationit was filtered
8. customall solvent was removed under reduced pressure