Reaction of boehmite, [AI(O)(OH)]n, with an excess of carboxylic acid (HO2CR) results in the formation of the carboxy substituted alumoxanes, [AI(O)x(OH)y(O2CR)z)]n where 2x + y + z = 3 and R = alkyl substituents. The alumoxanes have been fully characterized by SEM, elemental analysis, IR and multinuclear NMR spectroscopy. The physical properties of the alumoxanes are highly dependent on the identity of R, and range from insoluble crystalline powders, e.g. R = CH3, to powders which readily form solutions or gels in hydrocarbon solvents, e.g. R = C5H11. All of the alumoxanes decompose under mild thermolysis to yield γ-alumina.