反应详情

Carbontetrachloride (CCl4, 300 mL) and the product of Example 1 (50.6 g, 0.26 mol) were added to a 1 L flask equipped with a N2 inlet The solution was stirred until all solid dissolved. N-bromo-succinimide (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 6 h with a 500 watt reflector spot lamp. An additional 0.5 eq (23.4 g) of NBS was added to the reaction, and refluxing was continued for 2 h. After cooling the reaction to room temperature, it was filtered and all solvent was removed under reduced pressure. Flash chromatography (15/85 EtOAc/Hex) provided 31.6 g (47%) of title product and 22.2 g (33%) of the title material of Example 2.

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