反应详情

温度

100 °C

To a flask containing ethyl 2-(6-chloropyridin-3-yl)acetate 208-1 (300 mg, 1.5 mmol), 2-fluoropyridin-4-ylboronic acid 205-4 (318 mg, 2.25 mmol), Pd(OAc)2 (17 mg, 0.075 mmoL), 2-dicyclohexylphosphino-2′,6′-dimethoxyybiphenyl (62 mg, 0.15 mmol), K3PO4 (800 mg, 9 mmol) under argon was added 2-butanol (1.5 mL). The reaction mixture was stirred at 100° C. for 10 hours. After cooled to room temperature, the mixture was diluted with ethyl acetate, washed with water and brine, dried over Na2SO4, and concentrated to dryness by rotary evaporation. The crude was purified by silica gel flash chromatography, eluted with 40% ethyl acetate in dichloromethane to give ethyl 2-(2′-fluoro-2,4′-bipyridin-5-yl)acetate 208-2 as a yellow solid. MS m/z 261.1 (M+1).

1. temperatureAfter cooled to room temperature
2. washwashed with water and brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated to dryness by rotary evaporation
5. customThe crude was purified by silica gel flash chromatography
6. washeluted with 40% ethyl acetate in dichloromethane