反应详情

Diethylphosphonoacetic acid tert-butyl ester (1.0 g, 4.0 mmol) was dissolved in N,N-dimethylformamide (1.4 and 60% sodium hydride (0.17 g, 4.4 mmol) was added at 0° C. After stirring at room temperature for 30 minutes, the reaction mixture was cooled again to 0° C., ethyl iodide (0.33 mL, 4.1 mmol) was added, and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate, washed successively with 0.5N hydrochloric acid, water and saturated brine, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane=57/43) to give the title compound (0.92 g, 3.3 mmol, 83%).

1. additionwas added at 0° C
2. temperaturethe reaction mixture was cooled again to 0° C.
3. stirringthe mixture was stirred at room temperature overnight
4. washwashed successively with 0.5N hydrochloric acid, water and saturated brine
5. concentrationconcentrated under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane=57/43)