反应详情

温度

80 °C

To a stirred solution of 3-oxo-3-phenylpropanenitrile (1.5 g, 10.3 mmol) and NaOH (452 mg, 11.3 mmol) in water (10 mL)/EtOH (10 mL) was added hydroxylamine hydrochloride (785 mg, 11.3 mmol). The mixture was stirred at 80° C. for overnight. At this point, conc. HCl (1.3 mL, 15.5 mmol) was added and the resulting mixture was heated at 80° C. for 2 h. It was then basified to pH 10 and extracted with ethyl acetate. The combined extract was concentrated under reduced pressure and the residue was purified by silica-gel column chromatography eluting with ethyl acetate/petroleum ether (1:50 to 1:10) to afford 299a as a yellow solid (1.1 g, 68%). MS-ESI: [M+H]+ 161.3.

1. temperaturethe resulting mixture was heated at 80° C. for 2 h
2. extractionextracted with ethyl acetate
3. extractionThe combined extract
4. concentrationwas concentrated under reduced pressure
5. customthe residue was purified by silica-gel column chromatography
6. washeluting with ethyl acetate/petroleum ether (1:50 to 1:10)