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Ultrafine copper and nickel powders are synthesized by a chemical reduction of the metal cations from their salts in an aqueous ethanol solution without and with the addition of a polymer stabilizer (polyvinylpyrrolidone and polyvinyl alcohol). The structure and morphological features of the prepared metal powders were investigated by X-ray phase analysis and electron microscopy. The electrocatalytic properties of the Cu and Ni powders have been studied in the electrohydrogenation of acetophenone, nitrobenzene, p-nitroaniline, and cyclohexanone. A higher electrocatalytic activity of Cu powders, as well as skeletal copper, was established in the electrohydrogenation of the first three of the listed compounds in comparison with nickel powders, which is explained by the ability of copper cations to be reduced from its oxides in the electrochemical system under investigation. It is shown that the use of polymer stabilizers in the synthesis of Cu and Ni powders contributes to reducing metal particle sizes, but does not increase the electrocatalytic activity of the corresponding metal powders.