反应详情

温度

100 °C

564 g (6 mol) of ethylphosphonous acid are dissolved in 860 g of water and initially charged to a 5 l five-neck flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel. After heating the reaction mixture to 100° C., 602 g (7 mol) of vinyl acetate and 500 g of a 5% strength sodium peroxodisulfate solution (1.5 mol % based on vinyl acetate) are added dropwise at atmospheric pressure over 1 h. The water is then distilled off in vacuo. The residue is taken up in tetrahydrofuran and the insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo. Chromatographic purification leaves 1.026 g (95% of theory) of ethyl-(2-acetoxyethyl)phosphinic acid being obtained as an oil.

1. additioninitially charged to a 5 l five-neck flask
2. customequipped with thermometer
3. temperaturereflux condenser, high-performance stirrer
4. distillationThe water is then distilled off in vacuo
5. filtrationthe insoluble salts are filtered off
6. customThe solvent of the filtrate is removed in vacuo
7. customChromatographic purification