This paper describes the synthesis of nanocrystalline magnetic spinel CuFe2O4 via co-precipitation method and their catalytic application. The structural, morphological and magnetic properties of the nanocrystals were characterized by powder X-ray diffraction, Fourier transformed infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The powder X-ray diffraction results unveiled the crystal structure and spinel phase of CuFe2O4 with the average diameter size of 37.47 ± 4.92 nm. The FTIR spectra revealed the vibration bands of Cu–O and Fe–O at 464 and 572 nm respectively. The VSM result shows the nanoparticles exhibit superparamagnetic behavior. Thereafter, an efficient magnetic nanocatalyst CuFe2O4 (M/nanocat-CuFe2O4) have been used for the O-arylation of phenol with aryl halide under ligand-free conditions and K2CO3 as the base in DMF at 110 °C to produce biaryl ether. Structural characterization was done by FTIR and nuclear magnetic resonance spectroscopy. Moreover, The CuFe2O4 nanocatalyst was recovered by magnetically separation from the reaction mixture and reused several times with high catalytic activity.