反应详情

温度

50 °C

To a mixture of methyl 6-(2,6-difluorophenyl)-5-fluoropyridine-2-carboxylate (210.2 mg, 0.7867 mmol) and lithium hydroxide, monohydrate (162 mg, 3.86 mmol), THF (3.0 mL) was added followed by water (1.0 mL). The mixture was heated at 50° C. for 3 h. The reaction mixture was then cooled to 0° C., and 1 M HCl was added slowly until the pH reached 2. The reaction mixture was then diluted with water (20 mL), extracted with EtOAc (3×20 mL) and the combined organic layers were washed with brine (30 mL), dried over Na2SO4, and concentrated under reduced pressure to yield the sub-title compound as a white solid (162.1 mg, 81%). LCMS calc. for C12H7F3NO2 (M+H)+: m/z=254.0. found 254.0.

1. additionwas added
2. temperatureThe reaction mixture was then cooled to 0° C.
3. extractionextracted with EtOAc (3×20 mL)
4. washthe combined organic layers were washed with brine (30 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure