Abstract <p>This study reports the synthesis and characterization of Poly(<i>N</i>-methyl pyrrole) (PNMPy) and its nanocomposite with molybdenum trioxide (MoO₃) prepared via a chemical oxidative in situ polymerization method. The structural, optical, and electrical properties of the synthesized materials were investigated using Fourier Transform Infrared (FTIR) spectroscopy, X-ray diffraction (XRD), UV–Visible (UV–Vis) spectroscopy, and dielectric measurements. FTIR and XRD analyses confirmed strong interfacial interactions and homogeneous dispersion of MoO₃ within the PNMPy matrix, forming an ordered hybrid structure. The UV–Vis spectra revealed absorption bands at 380 and 500 nm, corresponding to π–π* and <i>n</i>–π* transitions, with a redshift indicating charge transfer between the polymer and oxide phases. The optical band gap of the PNMPy/MoO₃ nanocomposite (2.05 eV) was significantly lower than that of pure PNMPy (3.28 eV) and MoO₃ (≈3.0 eV), demonstrating enhanced electronic coupling. Dielectric studies showed that the PNMPy/MoO₃ nanocomposite exhibited semiconductor behavior with an electrical conductivity of 1 × 10^‒5&#xa0;S/m and an activation energy of 9.94 × 10^–2 eV. These findings indicate that the incorporation of MoO₃ nanoparticles effectively enhances the optical and electrical performance of PNMPy, making the composite a promising candidate for use in optoelectronic, sensing, and energy storage applications.</p>