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The H5PV2Mo10O40 catalyzed the oxidation of thiols to their homo- disulfides using hydrogen peroxide as the oxidant under mild conditions is reported. This system provides an efficient, convenient and practical method for the syntheses of symmetrical disulfides. In this work, comparisons of Keg- gin and Dawson type polyoxometalates are addressed in term of relative sta- bility, hardness and acidity.

H5PV2Mo10O40 as an efficient catalyst for the oxidation of thiols to the corresponding disulfides using hydrogen peroxide as the oxidant