反应详情

12.1 g of methyl 2-chloro-4-methanesulfonyl-3-methylbenzoate was dissolved in 250 ml of carbon tetrachloride, and the solution was refluxed under stirring. Then, 7.5 g of bromine and 1 g of benzoyl peroxide were gradually added thereto over a period of 30 minutes, and the solution was further refluxed for 4 hours under heating. After cooling, 200 ml of chloroform was added thereto, and the mixture was washed with a 5% sodium hydrogensulfite aqueous solution. The organic layer was separated and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain a crude product. The crude product was washed with ethyl ether to obtain 13.2 g of crystals of the desired product. Melting point: 77°-78° C.

1. temperaturethe solution was refluxed
2. temperaturethe solution was further refluxed for 4 hours
3. temperatureunder heating
4. temperatureAfter cooling
5. washthe mixture was washed with a 5% sodium hydrogensulfite aqueous solution
6. customThe organic layer was separated
7. dry with materialdried over anhydrous sodium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. customto obtain a crude product
10. washThe crude product was washed with ethyl ether