反应详情

A solution of 3-(3-bromo-4-methylphenyl)-5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole (1.2 g), N-bromosuccinimide (0.54 g) and 2,2′-azobisisobutylonitrile (0.05 g) in dichloroethane (20 mL) was heated to reflux for 3 hours. The solvent was distilled off under reduced pressure, the residue was diluted with t-butylmethylether, and the solution was washed with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel chromatography to yield 3-[3-bromo-4-(bromomethyl)-phenyl]-5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole (1.0 g).

1. temperatureto reflux for 3 hours
2. distillationThe solvent was distilled off under reduced pressure
3. additionthe residue was diluted with t-butylmethylether
4. washthe solution was washed with water and saturated brine
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by silica gel chromatography