反应详情

To a solution of 4-(3-phenylureido)benzoic acid (13.5 g, 52.68 mmol) in acetonitrile (250 mL) at room temperature was added tert-butyl piperazine-1-carboxylate (11.8 g, 63.22 mmol), 1H-benzo[d][1,2,3]triazol-1-ol (21.1 g, 156.5 mmol, HOBT) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (30 g, 156.5 mmol, EDCl). The mixture was stirred at reflux temperature for 16 hours and was then concentrated under vacuum. The residue was submitted to silica chromatography (0-5% ethyl acetate in n-hexanes as eluant) to give the title compound (15.0 g). MS (ESI) m/z 425.1 [M+H]+

1. temperatureat reflux temperature for 16 hours
2. concentrationwas then concentrated under vacuum