反应详情

To a solution of 8.5 g (0.03 mol) of 4-[4-(phenylmethyl)-1-piperazinyl]benzeneamine and 16.0 g (0.16 mol) of triethylamine in 450 mL of ethyl acetate was added, dropwise, a solution of 2.5 g (0.035 mol) of acetyl chloride in 50 mL of ethyl acetate. The mixture was magnetically stirred for 3 h and then heated at reflux for 1 h. The excess acetyl chloride was co-distilled with benzene and the resulting oil was shaken in 400 mL of 10% sodium hydroxide solution. The suspended tan solid was collected by filtration, washed thrice with 100 mL portions of water, and air dried to give 9.7 g (99%) of crude product. A one-gram portion was recrystallized from benzene/petroleum ether to give 100 mg of cream colored solid, mp 159°-161° C.

1. temperatureheated
2. temperatureat reflux for 1 h
3. filtrationThe suspended tan solid was collected by filtration
4. washwashed thrice with 100 mL portions of water, and air
5. customdried