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The interaction of tri-n-butylmethylphosphonium dimethylphosphate with elemental sulfur was described. The reaction products are isolated and characterized with 1H, 13C, 31P and 17O NMR spectroscopy. It is shown that dimethyl phosphateanion is active in the reaction, and the addition of sulfur atoms occurs through the oxygen atom of dimethyl phosphate-anion. It is found that a mixture of products, which differ in the number of sulfur atoms in the chain, is formed The assumptions were made about the mechanism of interaction of sulfur with tri-n-butylmethylphosphonium dimethylphosphate.