The present study aimed to evaluate the feasibility of developing low-cost N- and Fe-doped TiO₂ photocatalysts for investigating the mineralization of 2,4-dimethylaniline (2,4-DMA). With a single anatase phase, the photocatalysts showed high thermal stability with mass losses of less than 2%. The predominant oxidative state is Ti⁴⁺, but there is presence of Ti³⁺ associated with oxygen vacancies. In materials with N, doping was interstitial in the NH₃/NH⁴⁺ form and for doping with Fe, there was a presence of Fe-Ti bonds (indicating substitutional occupations). With an improved band gap energy from 3.16 eV to 2.82 eV the photoactivity of the photocatalysts was validated with an 18 W UVA lamp (340–415 nm) with a flux of 8.23 × 10⁻⁶ Einstein s⁻¹. With a size of only 14.45 nm and a surface area of 84.73 m² g⁻¹, the photocatalyst doped with 0.0125% Fe mineralized 92% of the 2,4-DMA in just 180 min. While the 3% N photocatalyst with 12.27 nm had similar performance at only 360 min. Factors such as high surface area, mesoporous structure and improved E_bg, and absence of Fe peak in XPS analysis indicate that doping with 0.0125% Fe caused a modification in TiO₂ structure.