376587-52-9

3430-18-0

376587-52-9

2,5-Dibromo-3-methylpyridine (M-12) (5.02 g, 20.0 mmol) was used as a raw material and dissolved in acetonitrile (50 mL). Subsequently, sodium iodide (12.0 g, 80.0 mmol) and acetyl chloride (2.85 mL, 40.0 mmol) were sequentially added to this solution. The reaction mixture was heated and stirred under reflux conditions for 24 hours. Upon completion of the reaction, it was cooled to room temperature, diluted with an appropriate amount of water and the pH was adjusted to 8 with saturated aqueous sodium bicarbonate solution to neutralize the reaction mixture. Extraction was carried out with ethyl acetate, the organic layer was collected and dried over anhydrous sodium sulfate, and the desiccant was removed by filtration. The solvent was removed by concentration under reduced pressure and the resulting residue was purified by silica gel column chromatography (eluent ratio: n-hexane/ethyl acetate=98:2→70:30) to afford the target product 5-bromo-2-iodo-3-methylpyridine (M-13) (5.76 g, 97% yield) as a red oil.