反应详情

温度

130 °C

To a solution of (3-bromo-4-fluoro-phenyl)-acetic acid (10 g, 42.9 mmol) in DMF (65 mL) was added copper (I) cyanide (7.7 g, 85.8 mmol) and heated at 130° C. for 24 hrs. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (250 mL). The organic layer was washed with water (5×50 mL), brine (50 mL), dried over sodium filtered and concentrated under reduced pressure. The crude material was re-crystallized from diethyl ether and hexane to afford the title compound as a yellow solid in 65% yield, 5 g.

1. temperatureThe reaction mixture was cooled to room temperature
2. washThe organic layer was washed with water (5×50 mL), brine (50 mL)
3. dry with materialdried over sodium
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe crude material was re-crystallized from diethyl ether and hexane