A novel core@double-shell three-layer structure with dendritic fibrous morphology based on Fe3O4@TEA@Ni–organic framework: a highly efficient magnetic catalyst in the microwave-assisted Sonogashira coupling reaction

Abstract

In synthetic organic chemistry, the formation of carbon–carbon bonds is a significant and substantial reaction. As a result, developing a highly active magnetic heterogeneous catalyst with excellent performance is a very appealing technique for constructing C–C bonds in organic chemistry. The present study describes the fabrication of a novel and readily recoverable nickel-based metal–organic framework (MOF) for C–C bond formation through the Sonogashira coupling reaction. The efficient magnetic core–shell structure (Fe₃O₄@TEA@MOF) with a 3D dendritic fibrous morphology was successfully synthesized using a hydrothermal approach by immobilizing Ni-based MOF onto the Fe₃O₄@TEA core–shell structure. The fabrication of Fe₃O₄@TEA@MOF was confirmed by various analyses; Fourier-transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray analysis (EDS), and elemental mapping confirmed the stepwise fabrication of catalyst. X-ray diffraction analysis (XRD) showed the crystalline nature of the catalyst. Field-emission scanning electron microscopy (FE-SEM) displayed the 3D dendritic fibrous morphology. Thermogravimetric analysis (TGA) and vibrating sample magnetometer analysis (VSM) showed the excellent thermal stability and magnetic properties of Fe₃O₄@TEA@MOF. The Brunauer–Emmett–Teller analysis (BET) found that the fabricated catalyst with a surface area of 36.2 m² g⁻¹, pore volume of 0.18 cm³ g⁻¹, and mean pore diameter of 20.38 nm belongs to mesoporous structures. In addition, the information from the inductively coupled plasma-optical emission spectroscopy (ICP-OES) about fresh and reused catalysts showed that the metal leaching amount is slight and about 1.98%. Other advantages of the Fe₃O₄@TEA@MOF catalyst can be mentioned as easily reusable for four runs and high performance (above 98%) in synthesizing diphenylacetylene from phenylacetylene, aryl halide, and cesium carbonate (as the base) under solvent-free and microwave conditions.