反应详情

温度

90 °C

To a solution of 2-bromo-6-(4-bromo-2,6-difluorobenzyl)pyridine (from Step C above, 7.41 g, 20.53 mmol) in toluene (200 mL) was added (2,4-difluorophenyl)boronic acid (3.89 g, 24.63 mmol), tetrakis(triphenylphosphine)palladium (2.37 g, 2.05 mmol), ethanol (20 mL) and 2M Na2CO3 (20 mL). The reaction was heated to 90° C. until complete. The mixture was cooled to room temperature and concentrated. The crude residue was diluted with EtOAc/water (1:1) and washed with 1N HCl (2×), brine (3×), dried over MgSO4, and concentrated in vacuo. The crude material was purified via silica gel chromatography (hexanes/ethyl acetate) to give the title compound (7.23 g).

1. temperatureThe mixture was cooled to room temperature
2. concentrationconcentrated
3. additionThe crude residue was diluted with EtOAc/water (1:1)
4. washwashed with 1N HCl (2×), brine (3×)
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customThe crude material was purified via silica gel chromatography (hexanes/ethyl acetate)