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The electrochemical polymerization of some Schiff's base‐type monomers like pyrrole‐2‐aldehyde azine, N,N′‐di(2‐pyrrolylmethylene)‐1,4‐diaminobenzene , and N,N′‐di(2‐pyrrolylmethylene)‐4,4′‐diaminobiphenyl proceeds as a precipitating polymerization to the anodic compartment. The voltammetric study of monomers and polymers using Pt electrodes and paste‐carbon electrodes were carried out. The results are in agreement with the MO calculations using the Hückel approximation for evaluating of the reactivity of the monomers.