反应详情

8.2 g of 4-chloro-3-nitro-benzoic acid-[N-(2-carboxy-ethyl)-amide](prepared from 4-chloro-3-nitro-benzoylchloride and β-alanine-methylester and subsequent saponification with 48% hydrobromic acid), 6.6 g of 2-(4-benzyl-piperazino)-ethylamine (prepared from 1-benzyl-piperazine and 2-bromo-ethylamine-hydrobromide in ethanol with the addition of potassium tert.butoxide), 4.2 ml of triethylamine and 25 ml of water are heated over a steam bath for 8 hours. The mixture is evaporated down and purified by column chromatography (silica gel; methylene chloride/methanol/glacial acetic acid=8:2:0.1 to 2:1:0.1). Yield: 9.2 g (67% of theory), Rf value: 0.47 (silica gel; methylene chloride/methanol/conc. ammonia=8:2:0.1)

1. temperatureare heated over a steam bath for 8 hours
2. customThe mixture is evaporated down
3. custompurified by column chromatography (silica gel; methylene chloride/methanol/glacial acetic acid=8:2:0.1 to 2:1:0.1)