反应详情

2-chloro-3-fluoro-5-methylpyridine in an amount of 4.00 g (27.6 mmol) was dissolved in 80 mL of carbon tetrachloride, following which 7.37 g (41.4 mmol) of N-bromosuccinimide and 20 mg of benzoyl peroxide were added and the mixture was refluxed overnight under heating. Following reaction completion, the reaction mixture was returned to room temperature, concentrated under reduced pressure, and purified by silica gel column chromatography (hexane/ethyl acetate=19:1), giving 3.06 g of 5-(bromomethyl)-2-chloro-3-fluoropyridine (yield, 51%).

1. additionwere added
2. temperaturethe mixture was refluxed overnight
3. temperatureunder heating
4. customreaction completion
5. customwas returned to room temperature
6. concentrationconcentrated under reduced pressure
7. custompurified by silica gel column chromatography (hexane/ethyl acetate=19:1)