反应详情

温度

80 °C

14.9 g of diethyl phenylmalonate was dissolved in 50 ml of N,N-dimethylformamide and 2.52 g of sodium hydride (60% oily) was added thereto at room temperature. Next, 5.0 g of 2-chloro-5-nitropyridine was added thereto and the resulting mixture was stirred at 80° C. for 2 hours. After the completion of the reaction, the reaction mixture was poured into ice-water/ethyl acetate and neutralized with dilute hydrochloric acid. After extracting with ethyl acetate, the extract was dried over anhydrous sodium sulfate and filtered. The filtrate was distilled under reduced pressure and the obtained residue was purified by silica gel column chromatography (eluted with ethyl acetate/n-hexane) to thereby give 16.55 g of the title compound as a reddish brown oily substance.

1. customat room temperature
2. customAfter the completion of the reaction
3. extractionAfter extracting with ethyl acetate
4. dry with materialthe extract was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. distillationThe filtrate was distilled under reduced pressure
7. customthe obtained residue was purified by silica gel column chromatography (eluted with ethyl acetate/n-hexane)