Solid State M-2-MeO-CP compounds, where M stands for bivalent metals (Mn, Fe, Co, Ni, Cu and Zn) and 2-MeO-CP is 2-methoxycinnamylidenepyruvate, were synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), elemental analysis and complexometry were used to establish the stoichiometry and to study the thermal behaviour of these compounds in CO and N atmospheres. The results were consistent with the general formula: M(L) ·H O. In 2 2 2 2 both atmospheres (CO , N ) the thermal decomposition occurs in consecutive steps which are characteristic of 2 2 each compound. For CO atmosphere the final residues were: Mn O , Fe O , Co O , NiO, Cu O and ZnO, while 2 3 4 3 4 3 4 2 under N atmosphere the thermal decomposition is still observed at 1000 º C.