反应详情

温度

-50 °C

Compound 1-4 (577 mg; 3.76 mmol) and potassium carbonate (779 mg; 5.64 mmol) were added to a solution of 2,4,6 trifluoropyridine (500 mg; 3.76 mmol) in DMF with stirring at −50° C. The reaction mixture was slowly warmed to room temperature and then diluted water and EtOAc, after which the aqueous layer was extracted with EtOAc. The combined organic layers were washed with water (3×), brine (2×), dried over MgSO4, and concentrated to an oil. The crude residue was purified via column chromatography (0-25% EtOAc in hexanes.) to give the title compound. MS M+1=266.9. 1H NMR (CDCl3): 6.32 (m, 2H), 7.30 (m, 1H), 7.36 (m, 1H), 7.56 (m, 1H).

1. temperatureThe reaction mixture was slowly warmed to room temperature
2. extractiondiluted water and EtOAc, after which the aqueous layer was extracted with EtOAc
3. washThe combined organic layers were washed with water (3×), brine (2×)
4. dry with materialdried over MgSO4
5. concentrationconcentrated to an oil
6. customThe crude residue was purified via column chromatography (0-25% EtOAc in hexanes.)