In recent years, the development of novel green chemistry routes for the synthesis of organic compounds has become very attractive to many research groups. Nanoparticles have been widely used because of their potential applications in catalysis, environmental remediation, electronic fields, biomedical, and industrial fields. In this article, a rapid, efficient, and simple approach was applied for the synthesis of 2,3‐diaminophenazine using a new photocatalytic system of CdFe2O4/TiO2 nanoparticles in water as a benign solvent. The structure of the synthesized CdFe2O4/TiO2 nanoparticle was confirmed using different methods such as transmission electron microscope (TEM), X‐ray diffraction (XRD), and magnetic measurements. It was found that the rate and yield of the photocatalytic synthesis of 2,3‐diaminophenazine were improved using CdFe2O4/TiO2 nanoparticles compared to other methods.