反应详情

温度

70 °C

To a stirred solution of diethyl 2-(2-fluoro-6-nitrobenzyl)malonate (146-2; 2.5 g, 0.0079 mol) in ethanol (30 mL) was added SnCl2.2H2O (8.9 g, 0.0395 mol) with constant stirring. The reaction mixture was heated at 70° C. for 0.5 h to 1 h. The reaction mixture was cooled to room temperature and then filtered through CELITE bed. The filtrate was basified with saturated Na2HCO3 solution and extracted with ethyl acetate (3×50 mL). The combined organic layer was washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated under vacuum to afford the title compound. MS (M+1): 284.1.

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered through CELITE bed
3. extractionextracted with ethyl acetate (3×50 mL)
4. washThe combined organic layer was washed with saturated aqueous sodium chloride solution
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated under vacuum