反应详情

温度

90 °C

30 g (201.2 mmol) 2-fluoro-5-formylbenzonitrile and 35 g (431.6 mmol) 3-aminocrotononitrile were dissolved in acetic acid (500 ml) and heated to 90° C. After 4 h, the reaction mixture was cooled to rt, concentrated, neutralized with a saturated aqueous solution of sodium bicarbonate, and extracted with ethyl acetate. The organic extracts were combined, dried over sodium sulfate and concentrated under reduced pressure. The remaining solid was dissolved in ethyl acetate, and hexane was added. The precipitate was filtered off to afford the title compound (45 g, 80% of th.) as a pale yellow solid.

1. temperaturethe reaction mixture was cooled to rt
2. concentrationconcentrated
3. extractionextracted with ethyl acetate
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. dissolutionThe remaining solid was dissolved in ethyl acetate
7. additionhexane was added
8. filtrationThe precipitate was filtered off