Ethyl vinyl ether → Ethyl(2-ethoxyethyl)phosphinic acid

Participants

Reaction Conditions

Reaction Steps

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., 504 g (7 mol) of vinyl ethyl ether and 500 g of a 5% strength sodium peroxodisulfate solution (1.5 mol % based on vinyl ethyl ether) 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 953 g (82% of theory) of ethyl(2-ethoxyethyl)phosphinic acid being obtained as oil.

Provenance & Evidence