反应详情

3.10 g (0.01 mol) of 2-(4-acetamidobutyryl)-5-chlorohydrocinnamic acid and 1.70 g (0.011 mol) of 1,1'-carbonyldiimidazole are stirred at room temperature for 1 hour in 30 ml of tetrahydrofuran. Then, 1.2 ml (0.011 mol) of 1-methylpiperazine are added thereto at -70° and the mixture is left to warm to room temperature overnight. After concentration of the solution, the residue is extracted first with methylene chloride/2N hydrochloric acid and then with methylene chloride/concentrated aqueous ammonia solution, dried with sodium sulfate and the solvent is distilled in a vacuum. Chromatography on silica gel with methylene chloride-methanol (20:1) and crystallization from ethyl acetate/hexane gives N-[3-[4-chloro-2-[2-[(4methyl-piperazin-1-yl)carbonyl]ethyl]-benzoyl]propyl]acetamide as white crystals with melting point 126°-128°.

1. waitat -70° and the mixture is left
2. extractionAfter concentration of the solution, the residue is extracted first with methylene chloride/2N hydrochloric acid
3. dry with materialwith methylene chloride/concentrated aqueous ammonia solution, dried with sodium sulfate
4. distillationthe solvent is distilled in a vacuum
5. customChromatography on silica gel with methylene chloride-methanol (20:1) and crystallization from ethyl acetate/hexane