Palladium nanoparticles decorated on polyaniline coated carbon fiber paper electrode (Pd‐PANI/CFP) was employed for TEMPO ((2,2,6,6‐tetramethylpiperidin‐1‐yl)oxyl) mediated electrocatalytic oxidation of pyridyl methanol to pyridyl carboxaldehyde using cyclic voltammetry in aqueous acidic media using a surfactant. The electrochemical properties of the modified electrodes were studied by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The physicochemical properties of the modified electrodes were studied using Scanning electron microscopy (SEM) with Energy dispersive X‐ray spectroscopy (EDS), Transmission electron microscopy (TEM), Optical profilometry, X‐ray diffraction (XRD) spectroscopy, Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. Pd‐PANI/CFP electrode has exhibited enhanced electrocatalytic activity towards TEMPO mediated oxidation of pyridyl methanol owing to higher electrochemically active surface area of the modified electrode. CV studies suggested higher electrochemical activity for Pd‐PANI/CFP electrode when compared to PANI/CFP and bare CFP electrodes towards TEMPO mediated oxidation of pyridyl methanol.