反应详情

温度

50 °C

20.2 g (114 mmol) of N-bromosuccinimide was charged to a N,N-dimethylformamide (DMF) 15 ml solution of 7.2 g (46 mmol) of 5-chloro-2-methoxy-4-methylpyridine, followed by stirring at 50° C. for 20 hours. A diluted sodium thiosulfate aqueous solution was added to the reaction solution, and the aqueous layer was extracted with diethyl ether. The organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate and subjected to filtration on the pad of a silica gel cake, and the solvent was distilled off under reduced pressure to obtain 10.6 g (yield: 97%) of 3-bromo-5-chloro-2-methoxy-4-methylpyridine (melting point: 44 to 45° C.).

1. extractionthe aqueous layer was extracted with diethyl ether
2. washThe organic layer was washed with a saturated sodium chloride solution
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationsubjected to filtration on the pad of a silica gel cake
5. distillationthe solvent was distilled off under reduced pressure