A novel azo dye based on sulfathiazole and resorcinol was successfully synthesized through diazotization followed by an azo-coupling reaction. The structural features of the synthesized compound were confirmed using FT-IR, 1H NMR, and mass spectrometric analyses. The photophysical behavior of the dye was examined by UV–visible spectroscopy in various solvents, revealing notable solvent-dependent absorption characteristics. In addition, fluorescence studies were carried out in different solvent media to evaluate the emissive properties of the dye. The electrochemical behavior of the azo compound was investigated at a glassy carbon electrode (GCE) using cyclic voltammetry. The voltammetric response exhibited two distinct cathodic reduction peaks corresponding to the stepwise reduction of the azo group. Furthermore, the linear dependence of peak current on scan rate suggested that the electrode process is predominantly adsorption-controlled. The strong interaction between the azo dye and the electrode surface indicates its promising applicability in electrochemical and sensing-related fields.