反应详情

温度

95 °C

To a solution of 3-[(6-bromopyridin-2-yl)methyl]-4-fluorobenzonitrile (from Step B above, 8.34 g, 28.6 mmol) in toluene (300 mL) was added (2,4-difluorophenyl)boronic acid (8.15 g, 34.4 mmol), tetrakis(triphenylphosphine)palladium (1.65 g, 1.40 mmol), ethanol (30 mL), and 2M Na2CO3 (30 mL). The resulting mixture was heated to 95° C. for 2 hours. The reaction was cooled to room temperature and filtered through celite and concentrated in vacuo. The crude residue was dissolved in EtOAc, washed with H2O, brine (2×), dried over MgSO4, and concentrated. The crude material was purified via silica gel chromatography (hexanes/ethyl acetate) to give the title compound as a white solid (7.03 g).

1. temperatureThe reaction was cooled to room temperature
2. filtrationfiltered through celite and
3. concentrationconcentrated in vacuo
4. dissolutionThe crude residue was dissolved in EtOAc
5. washwashed with H2O, brine (2×)
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customThe crude material was purified via silica gel chromatography (hexanes/ethyl acetate)