反应详情

BBr3 (20 mL, 0.211 mol) was added to 3-fluoro-4-methoxybenzonitrile (15.6 g, 0.103 mol) in dichloromethane (100 mL) at 0° C. Stirring was continued under reflux for 3 days under a nitrogen atmosphere. The reaction mixture was quenched with ice water and extracted with dichloromethane. The organic layer was washed with water and brine and then dried over sodium sulfate. Solvent evaporation under reduced pressure gave 13.3 g (94%) of the subtitle compound as a gray solid. 1H NMR (400 MHz, CDCl3) δ 7.38-7.42 (m, 2H), 7.09 (dd, J=8.8 Hz, 8.4 Hz, 1H), 5.68 (s, 1H).

1. temperatureunder reflux for 3 days under a nitrogen atmosphere
2. customThe reaction mixture was quenched with ice water
3. extractionextracted with dichloromethane
4. washThe organic layer was washed with water and brine
5. dry with materialdried over sodium sulfate
6. customSolvent evaporation under reduced pressure