反应详情

Into 4 ml of dimethylformamide, 0.65 g (2.2 mmol) of (E) 3-(2-aminophenyl)-2-methyl-2-propenoic acid p-nitrophenyl ester and 0.69 g (4.4 mmol) of 2-naphtylamine (manufactured by Aldrich Chemical Co., Inc.) were dissolved; and, with 0.36 ml of triethylamine (manufactured by Wako Pure Chemical Industries, Ltd.) being added thereto, the mixture was reacted at room temperature for 20 hours. After the completion of the reaction was verified by TLC, ethyl acetate and water were added to the mixture. The resulting ethyl acetate layer was fractionated, and was washed several times with a 5% aqueous sodium hydrogencarbonate solution and then with a saturated aqueous sodium chloride solution. After the washed solution was dried with magnesium sulfate anhydride, the solvent was evaporated under a reduced pressure, whereby a crude product was obtained. This product was refined by a silica gel column chromatography (developing solvent: methylene chloride/methanol=95/5), whereby 1.39 g of the aimed compound were obtained (yield: quantitative).

1. customthe mixture was reacted at room temperature for 20 hours
2. additionwere added to the mixture
3. washwas washed several times with a 5% aqueous sodium hydrogencarbonate solution
4. dry with materialAfter the washed solution was dried with magnesium sulfate anhydride
5. customthe solvent was evaporated under a reduced pressure, whereby a crude product
6. customwas obtained