反应详情

温度

120 °C

To a sealed tube were added 5-bromo-2-iodobenzonitrile 206-1 (500 mg, 1.6 mmol), 2-fluoropyridin-4-ylboronic acid 205-4 (229 mg, 1.6 mmol), Pd(PPh3)4 (94 mg, 0.08 mmol), Na2CO3 (516 mg, 4.9 mmol), toluene (2 mL), H2O (2 mL) and ethanol (0.5 mL). The reaction mixture was stirred at 120° C. overnight. After cooling to room temperature, the solvents were evaporated and the residue was redissolved in water (5 ml) and extracted with ethyl acetate (8 mL×3). The combined organic phases were dried over Na2SO4, and concentrated. The residue was purified by silica gel flash chromatography and eluted with 15% ethyl acetate in hexane to give 5-bromo-2-(2-fluoropyridin-4-yl)benzonitrile 206-3. MS m/z 277.1 (M+1).

1. temperatureAfter cooling to room temperature
2. customthe solvents were evaporated
3. dissolutionthe residue was redissolved in water (5 ml)
4. extractionextracted with ethyl acetate (8 mL×3)
5. dry with materialThe combined organic phases were dried over Na2SO4
6. concentrationconcentrated
7. customThe residue was purified by silica gel flash chromatography
8. washeluted with 15% ethyl acetate in hexane