Products of reductive and non-reductive methylation of two high-sulphur coals (Mequinenza and Illinois No. 6) have been extracted by dichloromethane. It has been established that the efficiency of the transformation of coal to the products soluble in CH2Cl2 is higher for coals subjected to non-reductive methylation by the Liotta method than for those after reduction in the potassium/liquid ammonia system. The extracts and the extraction residues were subjected to elemental analysis, IR spectroscopy, and AP-TPR (Atmospheric Pressure-Temperature Programmed Reduction) measurements. It has been shown that the main species undergoing extraction by CH2Cl2 are aliphatic compounds or aromatic structures of low degree of condensation. The effect of the extraction on the sulphur groups in coal has been discussed.