In the present study, cellulose@SP@catechin@Fe3O4 nanocomposite underwent synthesis and characterization employing various analytical techniques, including Fourier transform‐infrared spectroscopy (FT‐IR), field‐emission scanning electron microscopy, transmission electron microscopy, Brunauer–Emmett–Teller analysis, thermogravimetric analysis, vibrating sample magnetometry, X‐ray powder diffraction, and X‐ray spectroscopy. This reusable and efficient nanocomposite facilitated the synthesis of azo‐linked 4‐arylidene‐benzodiazepine, resulting in products with high yields. Characterization of these products was conducted utilizing 1H nuclear magnetic resonance (NMR), 13C NMR, and FT‐IR spectral data alongside mass analyses. Additionally, their antioxidant activities were assessed via 1,1‐diphenyl‐2‐picrylhydrazyl analysis.