Oxygen in basic solution has been used to oxidize Pocahontas No. 3 coal to a mixture of aromatic carboxylic acids, and copper(I) oxide in N-methylpyrrolidinone-quinoline has been used to decarboxylate the acids to provide a mixture of hydrocarbons. Most pendant alkyl groups have been removed in this sequence and the product distribution is much less complex than the product distributions that are obtained in direct oxidation reactions or in the analysis of coal liquids and extracts. Approximately 25% of the aromatic carbon atoms are retained in the products. The structures of these compounds have been investigated by gas chromatography-mass spectrometry and by high-resolution and laser desorption mass spectrometry. Approximately 150 compounds were detected in the GCMS experiments including a broad array of bi-, ter-, and quateraryls, fluorene and fluoranthene derivatives, polycyclic aromatic hydrocarbons with four, five, and six rings, dibenzo-and dinaphthofurans, and dibenzo- and dinaphthothiophenes. High-resolution mass spectrometry provided additional evidence concerning the principal products and extended the mass range to approximately 400 Da. Laser desorption work revealed that even larger molecules were present in the reaction products with distinct signals at 550 Da and definite intensity extending to 1200 Da. These results are compatible with many other results that have been obtained in the past decade and strongly infer that the relatively high-ranking Pocahontas No. 3 coal has many large, condensed, aromatic clusters that are methylated and connected through biaryl and heterocyclic linkages.