反应详情

2-Bromo-5-fluoroisonicotinic acid (500 mg, 2.27 mmol) was dissolved in ethanol (22.7 mL), and the solution was stirred under heat and reflux for 1 hour after adding thionyl chloride (0.829 mL, 11.3 mmol). The solvent was then evaporated under reduced pressure. The residue was extracted with chloroform after adding a sodium hydrogen carbonate aqueous solution. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=100/0→4/1) to give ethyl 2 bromo-5-fluoroisonicotinate (434 mg, yield 77%).

1. temperatureunder heat
2. temperaturereflux for 1 hour
3. customThe solvent was then evaporated under reduced pressure
4. extractionThe residue was extracted with chloroform
5. additionafter adding a sodium hydrogen carbonate aqueous solution
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. customthe solvent was then evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=100/0→4/1)