反应详情

A mixture of 0.8 g of 3-(3-pyridyl)-2-ethylacrylic acid, 2.2 g of 4-(4-diphenylmethyl-1-piperazinyl)butylamine, 0.87 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride, and 30 ml of dichloromethane is stirred at room temperature overnight. The reaction mixture is washed with water and dried over magnesium sulfate, and the solvent is distilled off. The residue is chromatographed on silica gel with chloroform-methanol (30:1) to give a brown oil, which is dissolved in 5 ml of ethanol containing 1.0 g of fumaric acid. To the resulting solution is added 15 ml of diethyl ether, and the solid separated is collected to give 1.4 g of the title compound. m.p. 137°-141° C. (recrystallized from ethanol-diethyl ether)

1. washThe reaction mixture is washed with water
2. dry with materialdried over magnesium sulfate
3. distillationthe solvent is distilled off
4. customThe residue is chromatographed on silica gel with chloroform-methanol (30:1)
5. customto give a brown oil, which
6. customthe solid separated
7. customis collected