This study investigates heterogeneous Ti–Si-based catalysts for the selective oxidation of organic compounds using hydrogen peroxide as a green oxidizing agent. The catalysts were synthesized via a hydrothermal sol–gel method, with carefully controlled conditions to ensure the effective incorporation of titanium species into the silica matrix, forming a highly ordered porous framework. A range of characterization techniques, including X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), UV–Vis diffuse reflectance spectroscopy (UV–Vis DRS), nitrogen adsorption–desorption (BET), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), was employed to analyze the physicochemical and structural properties of the materials.