反应详情

温度

120 °C

A mixture of formamidine hydrochloride (4.02 g, 49.9 mmol) and diethyl ethoxymethylenemalonate (5 ml, 24.95 mmol) in ethanol (4.99 ml) was heated to 120° C. (by microwave irradiation) for 15 h. After the reaction mixture was cooled to room temperature, ethyl acetate, hydrochloric acid (1M), and water were added. The aqueous layer was washed with ethyl acetate and then extracted with 3:1 chloroform:isopropanol. The combined organic extracts were dried over magnesium sulfate and concentrated under reduced pressure to afford ethyl 6-oxo-1,6-dihydropyrimidine-5-carboxylate as an orange solid. LRMS (ESI) calc'd for (C7H9N2O3) [M+H]+, 169.1; found 169.1.

1. custom(by microwave irradiation) for 15 h
2. temperatureAfter the reaction mixture was cooled to room temperature
3. washThe aqueous layer was washed with ethyl acetate
4. extractionextracted with 3:1 chloroform
5. dry with materialThe combined organic extracts were dried over magnesium sulfate
6. concentrationconcentrated under reduced pressure