反应详情

105 g (0.48 mol) of 13 and 90 g (0.5 mol) of N-bromosuccinimide were dissolved at room temperature in 2000 cm3 of carbon tetrachloride, admixed with 3 g of azobisisobutyronitrile and heated under reflux for 4 hours. The precipitated succinimide was filtered off, the solvent was removed under reduced pressure and the residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1). This gave 112 g (79%) of 14 as a colorless, lacrymatory oil.

1. temperatureheated
2. temperatureunder reflux for 4 hours
3. filtrationThe precipitated succinimide was filtered off
4. customthe solvent was removed under reduced pressure
5. filtrationthe residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1)