反应详情

10.8 g (0.045 mol) of methyl 2,3-dimethyl-4-methanesulfonylbenzoate was dissolved in 80 ml of carbon tetrachloride, and 8.3 g (0.047 mol) of N-bromosuccinimide and 0.1 g of benzoyl peroxide were then added, followed by stirring for 3 hours under heating reflux. After the solution was allowed to cool, insoluble substance was removed by filtration, and the resulting filtrate was washed with an aqueous sodium hydrogen bisulfite solution, and then dried over anhydrous magnesium sulfate. Next, the solvent was distilled off under reduced pressure, the residue was purified through silica gel column chromatography to obtain 6.2 g of methyl 3-bromomethyl-4-methanesulfonyl-2-methylbenzoate in a state of crystals. Yield=43.4%.

1. temperatureunder heating
2. temperaturereflux
3. temperatureto cool
4. custominsoluble substance was removed by filtration
5. washthe resulting filtrate was washed with an aqueous sodium hydrogen bisulfite solution
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationNext, the solvent was distilled off under reduced pressure
8. customthe residue was purified through silica gel column chromatography