Recently, there has been much interest in creating new layered transition metal oxides. Vanadium oxides may be used as sorbents, catalysts, and cathodes in lithium batteries. The modified sol-gel technique allows for some control towards the final structure of the compound. Using this technique, a new layered vanadium oxide compound - I, containing the surfactant dodecylphosphate, has been synthesized. After the removal of the organic ligand a new compound - II is formed which might be hexagonal. The compounds were analyzed using XRD, TGA, SEM, and NMR. VO2PO3(OH)C12H25(H2O)n is the general formula of the layered product I with a layer spacing of about 40 angstroms. II appears to be hexagonal with a = 43Å. The synthesis, composition, and structure of these compounds are discussed.