Ni‐Dimethylglyoxime complex immobilized on functionalized Fe3O4 was synthesized by a post‐grafting way and utilized as a novel, thermally stable, recoverable, and efficient for green synthesis of dicoumarols through reaction of 4‐hydroxycoumarin with various aldehydes in excellent yields and higher rate. Fe3O4@SiO2‐silylcyclopropyl‐dimethylglyoxime‐Ni superparamagnetic nanoparticles (MNPs) were investigated by Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X‐ray spectroscopy, X‐ray diffraction, vibrating sample magnetometer, and Brunauer–Emmett–Teller technique. This nanocatalyst could be conveniently recovered via the use of an external magnetic field and reused for subsequent reactions for at least 7 times without any remarkable change and decrease in catalytic activity.
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