FIELD: chemistry.
SUBSTANCE: trimethyl ether of phosphonoacetic acid is obtained by a reaction of interphase alkylation of dimethylphosphite by methylchloroacetate in a heterogenic system "organic phase/solid phase" in the presence of potassium carbonate with a molar ratio dimethylphosphite, methylchloroacetate and potassium carbonate, respectively, equal to (1-1.3):1:(1.5-2). Freshly distilled methylchloroacetate is added dropwise to the mixture of dimethylphosphite and potassium carbonate in multiple portions, optimally 3-6 equal portions every 2.5-3.5 hours. Synthesis is carried out for 10-18 hours with mixing the reaction mass at a rate of 300-450 revolutions per minute at a temperature of 20-50°C. To separate the target product the reaction mass is processed with a chloroform-water mixture, containing water in an amount from 1 to 3% by volume of the total mixture volume. After that, the reaction mass is filtered, a sediment is washed with chloroform, a filtrate is evaporated and the target product is separated by vacuum distillation.
EFFECT: method of obtaining trimethyl ether of phosphonoacetic acid is economical, energy-saving and environmentally friendly.
2 cl, 1 tbl, 14 ex
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Authors
Dates
2014-09-10—Published
2013-05-27—Filed