反应详情

2-Fluoropyridine-3-carboxylic acid (200 mg, 1.42 mmol) was dissolved in 2,2,2-trifluoroethanol (2 mL) and potassium tert-butoxide (477 mg, 4.25 mmol) was added. The mixture was then heated to 90 C for 4 h. The mixture was diluted with water (4 mL), 2M HCl was added to bring the solution to pH 4 and the mixture was extracted with DCM (3×4 mL). 2M HCl was added to the aqueous layer to bring the solution to pH 3 and the mixture was extracted with DCM (4×5 mL). The combined organic extractions were dried over sodium sulfate and evaporated under vacuum to afford the title compound (100 mg, 32%). Method C HPLC-MS: MH+ requires m/z=222. Found: m/z=222, Rt=1.17 min (100%).

1. temperatureThe mixture was then heated to 90 C for 4 h
2. additionwas added
3. extractionthe mixture was extracted with DCM (3×4 mL)
4. addition2M HCl was added to the aqueous layer
5. extractionthe mixture was extracted with DCM (4×5 mL)
6. extractionThe combined organic extractions
7. dry with materialwere dried over sodium sulfate
8. customevaporated under vacuum