反应详情

Into 20 ml of dichloromethane, 0.19 g (1.1 mmol) of (E) 3-(2-aminophenyl)-2-methyl-2-propenoic acid and 0.18 g of p-nitrophenol (manufactured by Wako Pure Chemical Industries, Ltd.) were dissolved; and 10 mg of dimethylaminopyridine (manufactured by Wako Pure Chemical Industries, Ltd.) were added thereto. While the mixture was stirred under cooling with ice, 0.41 g of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC-HCl) (manufactured by Wako Pure Chemical Industries, Ltd.) was added thereto in portions. The liquid was returned to room temperature and then was stirred for 20 hours. After the end point of this reaction was verified by TLC, the reaction liquid was concentrated under a reduced pressure and then was dissolved in 100 ml of ethyl acetate. This solution was washed several times with a 5% aqueous sodium hydrogencarbonate solution and then with a saturated aqueous sodium chloride solution, and was dried with magnesium sulfate anhydride. Further, the solvent was evaporated, whereby a crude product was obtained. This product was recrystallized from ethanol, whereby 0.29 g of the aimed product was obtained as a crystal (yield: 91%).

1. additionwas added
2. customwas returned to room temperature
3. stirringwas stirred for 20 hours
4. customthe reaction liquid
5. concentrationwas concentrated under a reduced pressure
6. dissolutionwas dissolved in 100 ml of ethyl acetate
7. washThis solution was washed several times with a 5% aqueous sodium hydrogencarbonate solution
8. dry with materialwith a saturated aqueous sodium chloride solution, and was dried with magnesium sulfate anhydride
9. customFurther, the solvent was evaporated
10. customwhereby a crude product was obtained
11. customThis product was recrystallized from ethanol