反应详情

1-(2′,4′-Dichloro-biphenyl-4-yl)-6-hydroxy-hexan-1-one (400 mg) was dissolved in a mixture of ethanol (10 mL) and water (5 mL). Hydroxylamine hydrochloride (300 mg) and sodium acetate (350 mg) were added and the mixture refluxed for 5 hours. After cooling, the mixture was diluted with water and extracted with ethyl acetate. Evaporation and recrystallisation from ether/petrol gave the title compound as a white solid. 13C NMR (CDCl3): δ 25.9, 26.2, 26.2, 32.3, 62.8, 126.1, 127.3, 129.6, 129.8, 132.0, 133.2, 134.0, 135.2, 138.4, 139.1 and 159.3. 1H NMR (CDCl3): δ 1.45 (2H, m), 1.59 (4H, m), 2.80 (2H, m), 3.62 (2H, m), 7.26 (2H, m), 7.41 (2H, d, J=7.0 Hz), 7.47 (1H, m) and 7.64 (2H, d, J=7.0 Hz).

1. temperaturethe mixture refluxed for 5 hours
2. temperatureAfter cooling
3. extractionextracted with ethyl acetate
4. customEvaporation and recrystallisation from ether/petrol