The straightforward co‐precipitation approach was used to effectively manufacture novel silica‐coated magnetic nanoparticles doped with cobalt (Co3O4). These nanoparticles were characterized using Field Emission Scanning Electron Microscopy (FE‐SEM), Energy‐Dispersive X‐ray Spectroscopy (EDS), Wavelength‐Dispersive Spectroscopy (WDX), Powder X‐ray Diffraction Spectroscopy (PXRD), Fourier transform infrared spectroscopy (FT‐IR), Thermo‐gravimetric Analysis (TGA), Inductive coupled plasma‐optical emission spectrometry (ICP‐OES), and Transmission Electron Microscopy (TEM), etc. Intriguingly, the catalytic performance of these nanocrystals for the amines, phenols, alcohols, and thiols acylation processes was examined in solvent‐free conditions, with outstanding yields. These nanoparticles were recycled at least 12 times without losing their catalytic activity.