At present, the use of heterogeneous catalysts together with environmentally friendly methodologies has been increasing for the synthesis of value-added products.[1] Schiff bases (SB) and their derivatives are very versatile compounds of great importance in the fine chemical industry since they are widely used in various chemistry fields such as, pharmaceutical, clinical, pharmacological, electrochemical, catalytic, photochemical and luminescence. [2-4] On the other hand, the use of mixed metal oxides (MMO) derived from hydrotalcites (LDHs) as catalysts has been increased in organic chemistry. In this work, we synthetized, characterized, and employed MMOs modified with Cu (II) and Ni (II) as catalyst in the synthesis of SB derived from 2-aminothizoles and aromatic aldehydes. The MMOs synthetized were labeled as NixMMO and CuyMMO (x and y, denotes the percentage of substitution of Mg (II) ions by Ni (II) or Cu (II) ions). The electrochemical behavior of these MMOs were determined by cyclic voltammetry and chronoamperometry using a system of three electrodes: Ag/AgCl electrode (reference electrode), Pt wire (counter electrode) and carbon paste electrode (CPE) modified with MMOs (working electrode) in an electrochemical cell. The analysis was carried out employing NaOH (0.1 mol L-1) and NaCl (0.05 mol L-1) as electrolytic. [5] The electrochemical behavior of these MMO were compared with the catalytic results obtained in the synthesis of SB determining the influence of the metal substituted on the catalysts.[1] Vargas, J. M., Henrique, L., Morelato, T., Ortega, J. O., Boscolo, M., & Metzker, G. (2020). Upgrading 1-butanol to unsaturated, carbonyl and aromatic compounds: a new synthesis approach to produce important organic building blocks. Green Chemistry, 22, 2365-2369[2] Muhammad, A. R., Necmi, Dege., Onur, E. D., Tuğgan, Ağar., & Sajjad, H. S. (2020). Synthesis of two new Schiff bases; crystal structure, Hirshfeld surface analysis, density functional theory and molecular docking. Molecular Structure, 1226, 129330.[3]Revenga, M., Robledo, S., Martínez, E., González, M., Colina, A., Herase, A., Parientea, F., & Lorenzo, E. (2020). Direct determination of monosaccharides in honey by coupling a sensitive new Schiff base Ni complex electrochemical sensor and chemometric tools. Sensors and Actuators B: Chemical, 312. 127848.[4] Maza, S., Kijatkin, C., Bouhidel, Z., Pillet, S., Schaniel, D., Imlau, M., Guillot, B., Cherouana, A., & Bendeif, E. (2020). Synthesis, structural investigation and NLO properties of three. Journal of Molecular Structure, 1219, 128492.[5] Aguilar, V., Gonzalez, I., & Valente, J. S. (2011). Comparative Electrochemical Study of MgZnGa and ZnGaAl Hydrotalcites. ECS Transactions, 36, 247–256.