反应详情

温度

90 °C

To a solution of 4-bromo-6-fluorobenzonitrile (5 g, 25 mmol) in anhydrous DMF (20 mL) was added Zinc cyanide (1.75 g, 14.9 mmol) and tetrakis(triphenylphosphine)-palladium(0) (0.6 g, 0.519 mmol). The reaction mixture was heated overnight under argon at 90° C. After cooling to room temperature, the reaction mixture was poured into ethyl acetate (150 mL) and extracted with water 50 mL, 2×30 mL, brine (30 mL), then dried over anhydrous sodium sulfate. After rotary evaporation of most solvent, the concentrated solution was loaded onto a silica column and eluted with EtOAc/Hexane (1:6). A white solid was obtained (3.73 g). 1H-NMR (300 MHz, CDCl3) δ 7.80 (m, 1H), 7.58 (m, 2H).

1. temperatureAfter cooling to room temperature
2. extractionextracted with water 50 mL, 2×30 mL, brine (30 mL)
3. dry with materialdried over anhydrous sodium sulfate
4. customAfter rotary evaporation of most solvent
5. washeluted with EtOAc/Hexane (1:6)
6. customA white solid was obtained (3.73 g)