反应详情

温度

80 °C

To a solution of 2-amino-5-fluorobenzonitrile (9.90 g, 72.8 mmol) in acetonitrile (200 mL) was added N-chlorosuccinimide (10.7 g, 80.1 mmol) in several portions. The reaction mixture was heated at 80° C. for 16 hours, then cooled and concentrated to approximately 100 mL under reduced pressure. The residue was poured into water (1 L), and the resultant precipitate was filtered, washed with water and dried (50° C. under vacuum) to give the title compound as a light brown solid (12.37 g, 100%). 1H NMR (300 MHz, CDCl3): δ 7.27 (dd, J=7.9, 2.9 Hz, 1H), 7.09 (dd, J=7.9, 2.9 Hz, 1H), 4.69 (br s, 2H).

1. temperaturecooled
2. concentrationconcentrated to approximately 100 mL under reduced pressure
3. additionThe residue was poured into water (1 L)
4. filtrationthe resultant precipitate was filtered
5. washwashed with water
6. customdried (50° C. under vacuum)