反应详情

温度

70 °C

To a solution of 2-(allyloxy)-1-(5-bromo-2-fluorophenyl)ethanone (118 g, 432.1 mmol) in ethanol (1.7 L) is added hydroxylamine hydrochloride (34.5 g, 496.9 mmol) and sodium ethanoate (40.8 g, 496.9 mmol) at 25° C. The reaction is heated at 70° C. for 1 hr. The reaction is cooled and the solvent is removed under reduced pressure. The residue is washed with water (1 L) and is extracted three times with dichloromethane (3×500 mL). The organic phase is dried over magnesium sulfate, filtered, and the solvent is removed under reduced pressure, to obtain the title compound as a mixture of two possible oximes (120 g, 96%). ES/MS m/e (79Br/81Br) 288, 290 (M+1).

1. temperatureThe reaction is cooled
2. customthe solvent is removed under reduced pressure
3. washThe residue is washed with water (1 L)
4. extractionis extracted three times with dichloromethane (3×500 mL)
5. dry with materialThe organic phase is dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent is removed under reduced pressure