Magnetic [FA‐c‐(C‐DTX)@Fe3O4] nanocomposites have been prepared with a four‐step technique involving three mechanical stirring conventional steps to obtain [(FA‐c‐(DTX‐g‐DAC)] and an ultrasound‐assisted Fe3O4 coating approach to fabricate [FA‐c‐(C‐DTX)@Fe3O4]. Magnetic nanoparticles (NPs) (Fe3O4 NPs) synthesis and integration has been easily and rapidly approached under novel environmentally friendly optimized reaction conditions: an ethanol–water solution, one iron precursor use, short reaction time, low temperature, and an ultrasonic irradiation process. This new condition's unique combination is attributed to our new synthesis procedure. Sonochemically synthetisized [FA‐c‐(C‐DTX)@Fe3O4] were easily separated from the reaction mixture simply via external magnetic field application, and therefore, neither filtration nor centrifigation was required. The synthetisized samples have been investigated by Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, X‐ray photoelectron spectroscopy (XPS), X‐ray diffraction (XRD), thermogravimetry analysis (TGA), scanning electron microscopy (SEM), and vibrating‐sample magnetometry (VSM). Obtained outcomes including successful magnetite coating process, good crystallinity, homogenous morphology, enhanced thermal stability, and obvious magnetic properties suggested the potential of sonochemical procedure to fabricate and integrate magnetic NPs. This sonochemically synthesized catalyst was evaluated toward the reduction of the organic pollutant 4‐nitrophenol and showed excellent catalytic activity. This ultrasound‐assisted nanocomposites preparation is simply scalable to meet industrial application.