反应详情

A mixture of 6-bromo-3-methyl-1,2-benzisoxazole (675 mg), N-bromosuccinimide (642 mg) and 1,1′-azobis(cyclohexanecarbonitrile) (90 mg) in carbon tetrachloride (7 ml) was irradiated using a 300W lamp at reflux under nitrogen for 40 h. On cooling the precipitate was removed by filtration, the solvent was evaporated and the residue was purified by flash chromatography on a silica column (4 cm diam) eluting with a cyclohexane-ethyl acetate gradient (49:1 to 24:1) to give the title compound as a pale yellow solid (350 mg).

1. customwas irradiated
2. temperatureat reflux under nitrogen for 40 h
3. temperatureOn cooling the precipitate
4. customwas removed by filtration
5. customthe solvent was evaporated
6. customthe residue was purified by flash chromatography on a silica column (4 cm diam)
7. washeluting with a cyclohexane-ethyl acetate