Abstract: The electro-hydrogenation of coal on Pb electrode in a mixed dimethylformamide-ethanol (DMF-EtOH) electrolyte was investigated. The hydrogenation product was in-situ extracted from the organic solvent and characterized. The electrolysis products show a significant increase in H/C ratio, indicating increased hydrogenation efficiency. IR spectroscopy shows the reduction of C=O bond and aromatic ring, as well as the cleavage of bridge bonds, such as C-O-C, are the main reactions during the electrolysis. This is also confirmed by the increase of γ-H content measured by ¹H-NMR.