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Organic thiocyanates are important synthetic intermediates to access valuable sulfur compounds. In this manuscript, two methods (A and B) will be presented for their preparation. Indeed, the thiocyanation agent used in our work was NH4SCN which is an important reagent for the production of this class of intermediates, in the presence of some natural and synthetic catalysts with the oxidizing agent K2S2O8 in methanol. We took phenol and indole as model substrates and the results obtained were very satisfactory.