(dipeptide)xV2O5.1.0H2O (0.27<x<0.37) precipitates have been synthesized by adding dipeptides (Val-Gln, Ala-Gln, Gly Gln, Gly Glu and Ala-Gly) to a metavanadate solution acidified using a proton exchange resin. As evidenced by X-ray diffraction, these vanadium oxides exhibit the layered structure of the V2O5.1.8H2O xerogels in which dipeptides are intercalated between the layers. These precipitates result from the assembly of ribbon like particles into a sponge like morphology as evidenced by scanning electron microscopy. The vanadium oxide phases were also characterized by 51V MAS NMR while 13C CP MAS NMR allowed to investigate the dipeptide preservation during the synthesis.