反应详情

2-Chloro-5-nitrobenzoic acid (179 g), 182.5 g 1-(2-aminoethyl)-4-phenylpiperazine, 138 g K2CO3, 900 ml isoamyl alcohol and CuO catalyst were refluxed for 8 hours adding a pinch of CuO periodically. The mixture was cooled overnight, diluted with butanol and filtered. The solid was dissolved in water and neutralized to pH 4-4.5 with 3N HCl to give 247 g crude product. This was recrystallized from 3.5 liters dimethylformamide and 1 liter of water to give 220 g product, m.243-6°.

1. additionadding a pinch of CuO periodically
2. temperatureThe mixture was cooled overnight
3. filtrationfiltered
4. dissolutionThe solid was dissolved in water and neutralized to pH 4-4.5 with 3N HCl
5. customto give 247 g crude product
6. customThis was recrystallized from 3.5 liters dimethylformamide and 1 liter of water