反应详情

To a mixture of N-[methylsulfanyl-(4-(pyridin-2-yl)piperazin-1-yl)methylene]-benzamide (2.9 g, 8.52 mmol) in pyridine (50 ml) was added N1-(4-bromobenzyl)-N1-(pyridin-2-yl)-propane-1,3-diamine (3 g, 9.37 mmol) and the reaction mixture was heated at reflux for 18 h. The volatiles were evaporated in vacuo and the residue dissolved in dichloromethane (100 ml) and evaporated in vacuo. The residue was purified by column chromatography on silica gel (600 ml) using first a mixture of ethyl acetate/triethylamine 95:5 (1 l) followed by a mixture of 20 ethyl acetate/methanol/triethylamine 90:5:5 as eluents affording 2.95 g of N-[[3-[N-(4-bromo-benzyl)-N-(pyridin-2-yl)amino]propylamino]-(4-pyridin-2-yl-piperazin-1-yl) methylene]benzamide as a foam.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux for 18 h
3. customThe volatiles were evaporated in vacuo
4. dissolutionthe residue dissolved in dichloromethane (100 ml)
5. customevaporated in vacuo
6. customThe residue was purified by column chromatography on silica gel (600 ml)
7. additiona mixture of ethyl acetate/triethylamine 95:5 (1 l)
8. additionfollowed by a mixture of 20 ethyl acetate/methanol/triethylamine 90:5:5 as eluents