Three new compounds with the general formula [MCu(C3H2O4)(2)(H2O)(n)] (M is Ca (n = 3), Sr and Ba (n = 4)) have been synthesized and characterized by analytical and infrared techniques. X-ray diffraction methods have shown that all the complexes have orthorhombic unit cells. Thermal decomposition of these compounds using TGA-DSC and DTA techniques involves three consecutive steps : dehydration, ligand pyrolysis and inorganic residue evolution. Dehydration is an endothermic process with enthalpies of around 200 kJ mol(-1). Kinetic analysis of the dehydration curves has been performed and the Johnson equation gave the best correlation factors for the three complexes. Further treatments in tubular furnaces resulted in the formation of mixed oxides of formula MCuO(2) (M is Ca, Sr and Ba). The formation of small homogeneous particles in these oxides, as with metallo-organic percursors, has been observed by scanning electron microscopy.