In this paper the preparation and characterization of modified electrodes based on carbon nanotubes / pyrrole / cobalt phthalocyanine was done to obtain hybrid materials for the electrochemical oxidation of 2-mercaptoethanol. To prepare these new electrodes, two steps were followed. First, single-walled CNT (SWNT) deposits were made in aqueous solution on glassy carbon (GC) to obtain GC/CNT electrodes. Subsequently, pyrrole (Py) was incorporated on the CNTs to produce GC/CNT/PPy electrodes by electropolymerization. Pyrrole electropolymerization was a useful method to control the film characteristics. Both deposits were studied using a redox model reaction with ferrocenemethanol (FeMeOH), enabling the determination of the stability and charge transfer characteristics of the obtained electrodes. Finally, CoPc was incorporated into the hybrid electrodes, and their response for the oxidation of 2-mercaptoethanol was investigated.