Intercalated group IVB-VIB metal disulfides and diselenides MX 2 (M = Ti, Zr, Nb, Mo) can be obtained by electrochemical reduction of the corresponding MX 2 in the presence of tetraalkylammonium salt. An original approach was used, which allowed effective reduction of these insoluble substances in the form of powders suspended in an organic solvent using the standard electrolysis technique in solutions in a one-space electrolyzer with a soluble anode. Using electron transfer mediators in the process afforded intercalated compounds with yields of 60–100%.