反应详情

温度

0 °C

Diethyl cyanomethylphosphonate (1.42 g) was dissolved in dimethylformamide (50 ml), and sodium hydride (0.32 g; 60% dispersion in mineral oil) was added thereto at 0° C. under cooling. After the foaming ceased, 3-chloro-4,5-dipropargyloxybenzaldehyde (2.00 g) was added to the reaction mixture, which was stirred at room temperature overnight, poured into ice-water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 2-(3-chloro-4,5-dipropargyloxyphenyl)acrylonitrile (1.85 g). m.p., 110°-111° C.

1. extractionextracted with ethyl acetate
2. washThe extract was washed with water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography