反应详情

Potassium tert-butoxide (954 mg, 8.51 mmol) was charged to a sealed tube with 2,2,2-trifluoroethanol (4 mL) and 3-fluoropyridine-2-carboxylic acid (400 mg, 2.84 mmol) and the mixture was heated to 130 C for 26 h, then to 150 C for 4 h, and then to 120 C for approximately 18 h. The mixture was diluted with water (6 mL) and washed with DCM (2×4 mL), which was then discarded. 1M HCl was added to bring the solution to pH 7 and the aqueous was extracted with DCM (2×4 mL). The extraction process was repeated as above at pH 5, 4 and 3. The combined organic extractions were dried over sodium sulfate and evaporated under vacuum to afford the title compound as a white solid (305 mg, 49%). Method B HPLC-MS: MH+ requires m/z=222. Found: m/z=222, Rt=0.73 min (100%).

1. temperaturethe mixture was heated to 130 C for 26 h
2. waitto 120 C for approximately 18 h
3. washwashed with DCM (2×4 mL), which
4. addition1M HCl was added
5. extractionthe aqueous was extracted with DCM (2×4 mL)
6. extractionThe combined organic extractions
7. dry with materialwere dried over sodium sulfate
8. customevaporated under vacuum