反应详情

A solution of benzophenone (10.0 g), hydroxylamine hydrochloride (10.0 g), pyridine (50 ml), and absolute ethanol (50 ml) was pumped through the CMR (15 ml/min; 155°-60° C., 700 kPa). The effluent was cooled and the solvent removed by rotary evaporation, and the residue stirred with cold water (50 ml). The crued oxime was filtered off and recrystallised from ethanol to afford pure product (8.0 g; 73% yield), m.p. 140.5°-141° C., cf lit.5 for a batchwise preparation by microwave heating.

1. customwas pumped through the CMR (15 ml/min; 155°-60° C., 700 kPa)
2. temperatureThe effluent was cooled
3. customthe solvent removed by rotary evaporation
4. filtrationThe crued oxime was filtered off
5. customrecrystallised from ethanol
6. customto afford pure product (8.0 g; 73% yield), m.p. 140.5°-141° C., cf lit.5
7. customfor a batchwise preparation by microwave
8. temperatureheating