反应详情

4'-Chloro-5-ethyl-2-hydroxybenzophenone (65.2g) and potassium hydroxide (170g) in water (700ml) and ethanol (150ml.) were treated with hydroxylamine hydrochloride (70.0g), with cooling, and the resulting mixture was stirred for 18 hours at ambient temperature. Dissolution occurred during this time. The solution was acidified with 5N-hydrochloric acid and then extracted with ether (3×200ml.). The combined ether solutions were washed with 10% aqueous sodium carbonate solution (2×200ml) and evaporated to dryness to give an off-white solid. This solid was recrystallised from 40% benzene/60-80 petrol ether to give a white crystalline solid (29.9g), second crop (14.5g.) m.p.117°C.

1. temperaturewith cooling
2. dissolutionDissolution
3. extractionextracted with ether (3×200ml.)
4. washThe combined ether solutions were washed with 10% aqueous sodium carbonate solution (2×200ml)
5. customevaporated to dryness
6. customto give an off-white solid
7. customThis solid was recrystallised from 40% benzene/60-80 petrol ether