The oxidative desulfurization of a straight-run, nonhydrotreated diesel fraction (boiling range 178-342A degrees C) containing benzothiophene, dibenzothiophene, their alkyl-substituted derivatives, and thioxanthene by the action of hydrogen peroxide in the presence of transition metal compounds (Na2MoO4, Na2WO4, NaVO3, WO3, tungstic acid, and heteropoly tungstate/molybdate H(3)PMo(6)W(6)O(4)0) in a biphasic system followed by the extraction of the oxidation products with dimethylformamide has been studied. The oxidation of the hydrocarbon fraction in the presence of heteropoly tungstate/molybdate under biphasic conditions provides for the removal of up to 82% of total sulfur.