Electropolymerization of carboxylated conducting polymer/carbon nanotubes (CNTs) composites thin films has been studied by in situ electrochemical-surface plasmon resonance (EC-SPR) spectroscopy. Two derivatives of benzothiophene, thianaphthene-2-carboxylic acid and benzothiophene-2-propionic acid, composited with CNTs were electropolymerized in an acetonitrile with the potential range between 0 and 1.2V at scan rate of 20mV/s. The obtained films were characterized by in situ EC-SPR spectroscopy, UV-vis absorption spectroscopy, and atomic force microscopy. It was found that CNTs can improve properties of polymer/CNT composites films. Moreover, the obtained thianaphthene-2-carboxylic acid film can be further used for construction of immunosensor for detection of human IgG.