反应详情

温度

45 °C

To a solution of ethyl 2,2-bis(4-fluorophenyl)acetate (1.55 g, 5.64 mmol) in anhydrous dioxane (10 mL) was added sodium ethoxide (0.38 g, 5.61 mmol), and the reaction was stirred at a temperature between 40-50° C. for 30 minutes. Acrylonitrile (0.35 mL, 5.61 mmol) was added dropwise with stirring, and the reaction was heated at 60-70° C. for an additional 1 hour. The dioxane was removed in vacuo, and the residue was taken up in ether, washed with water and brine, dried with MgSO4, filtered and concentrated. Silica gel chromatography eluting with a gradient of 3% to 10% ethyl acetate/hexane gave the title compound. MS (DCI) m/z 342 (M+NH4)+.

1. stirringwith stirring
2. temperaturethe reaction was heated at 60-70° C. for an additional 1 hour
3. customThe dioxane was removed in vacuo
4. washwashed with water and brine
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. washSilica gel chromatography eluting with a gradient of 3% to 10% ethyl acetate/hexane