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?

Nanoscale Pub Date: 2022-05-04 DOI: 10.1039/D2NR00303A

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.

Graphical abstract: 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
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