A novel heterocyclic azo dye was synthesized and characterized using FT-IR, 1H NMR, mass spectrometry, and UV–visible spectroscopy techniques. The electrochemical behavior of the synthesized azo compound was investigated using a carbon paste electrode in 0.1 M H2SO4 as the supporting electrolyte. In addition, the effects of pH, scan rate, and concentration on the electrochemical response were systematically studied. The investigated azo compound exhibited two irreversible reduction peaks corresponding to the reduction of the azo (–N=N–) group. The reduction process involved the transfer of four electrons and resulted in the cleavage of the azo linkage into amino groups. The electrode reaction was found to be diffusion-controlled. Keywords: Azo dye, carbon paste electrode, Cyclic Voltammetry.