反应详情

4.7 g of 1,4-dihydro-2,6-dimethyl-3,5-pyridinecarboxylate and 1.3 g of scandium triflate were added to 2.75 g of 4-acetylbenzaldehyde (18.56 mmol), 1.7 ml of morpholine and 3 g of 4 Å molecular sieves in 100 ml of tetrahydrofuran under argon, and the mixture was heated to reflux for 3 hours. The mixture was concentrated. The residue was mixed with ethyl acetate and washed with sat. NaHCO3 solution and sat. NaCl solution. Drying and evaporation of the mixture resulted in a crude product which was purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 40-80%). 1.85 g of a yellowish oil were obtained.

1. temperaturethe mixture was heated
2. temperatureto reflux for 3 hours
3. concentrationThe mixture was concentrated
4. additionThe residue was mixed with ethyl acetate
5. washwashed with sat. NaHCO3 solution and sat. NaCl solution
6. customDrying
7. customevaporation of the mixture
8. customresulted in a crude product which
9. customwas purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 40-80%)