Abstract: Two coals were oxidized with aqueous NaOCl solution under mild conditions. The reaction mixture acidified was sequentially extracted with ethoxyethane, CS₂, petroleum ether, acetic ester and benzene, followed esterification by CH₂N₂ and analysis with GC/MS. The results show that chloro-substituted compounds, aliphatic acids and aromatic polycarboxylic acids are main products. The oxidative product was sequentially extracted with different polar solvents and achieved a simple group separation. Effective separation and analysis of oxidation products of coal in aqueous NaOCl solution, established by the study, provides a feasible method for high value-added use of coal.