反应详情

Sodium (3.00 g, 130 mmol) was added in portions into 80 mL of methanol and the mixture was stirred for 20 min until the sodium was completely dissolved. Then 4-bromo-2-fluoro-3-methylbenzonitrile (8.00 g, 37.3 mmol) was added and the solution was refluxed for 4 hours before cooling down. The reaction mixture was poured into ice/water (300 mL) and the resulting precipitate was collected by filtration. The solid afforded was dried under reduced pressure at 40° C. to give 4-bromo-3-methyl-2-(methyloxy)benzonitrile. 1H-NMR (400 MHz, CDCl3) δ ppm 7.39 (d, J=8.0 Hz, 1H), 7.28 (d, J=8.0 Hz, 1H), 4.00 (s, 3H), 2.37 (s, 3H).

1. dissolutionwas completely dissolved
2. temperaturethe solution was refluxed for 4 hours
3. temperaturebefore cooling down
4. filtrationthe resulting precipitate was collected by filtration
5. customThe solid afforded
6. customwas dried under reduced pressure at 40° C.