反应详情

150 mg (0.416 mmol) of mono(2-cyanoethyl) 4-(3-chlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate and 81.4 mg (0.499 mmol) of 3-(2-methoxyphenyl)-allylamine were dissolved in 10 ml of dichloromethane. 120 mg (0.624 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 63.7 mg (0.416 mmol) of 1-hydroxybenzotriazole were added to the obtained solution under cooling with ice, and they were stirred at room temperature for 2 hours. Dichloromethane was evaporated under reduced pressure. Ethyl acetate was added to the residue, and the product was washed with 1 N hydrochloric acid and then with a saturated aqueous sodium hydrogencarbonate solution. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (dichloromethane/methanol=100/1) to obtain the title compound.

1. temperatureunder cooling with ice, and they
2. customDichloromethane was evaporated under reduced pressure
3. additionEthyl acetate was added to the residue
4. washthe product was washed with 1 N hydrochloric acid
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by the silica gel chromatography (dichloromethane/methanol=100/1)