NiII immobilized on aminated Fe3O4@TiO2 yolk-shell NPs functionalized by -3-glycidyloxypropyl-trimethoxysilane -Fe3O4@TiO2 YS-GLYMO-UNNiII- was prepared as a stable, highly efficient, and reusable magnetic nanostructured catalyst for the C-P cross coupling reaction. A variety of spectroscopic and microscopic techniques such as Fourier transform infrared -FT-IR- spectroscopy, X-ray diffraction -XRD- analysis, transmission electron microscopy -TEM-, field emission scanning electron microscopy -FE-SEM-, energy-dispersive X-ray spectroscopy -EDS-, EDS-map, thermogravimetric analysis -TGA-, vibrating sample magnetometry -VSM-, inductively coupled plasma atomic emission spectroscopy -ICP-AES- and CHNS analysis were used to characterize the synthesized nanostructured catalyst. The characterizations determined that the nanostructured catalyst is superparamagnetic in nature, structured as core-shell and its average particle size is 30-32 nm. The catalytic activity of this new magnetic nanostructured catalyst -Fe3O4@TiO2 YS-GLYMO-UNNiII- was examined in the C-P cross coupling reaction of aryl halides/ aryl boronic acids/ styrene/ phenylacetylene with diethylphosphite/ triethylphosphite in the presence of WERSA so that arylphosphonates/ vinylphosphonate/ alkynylphosphonate could be prepared in a short period of time. In all the cases, the nanostructured catalyst could be easily recovered magnetically for at least seven runs and a simple work-up procedure was used to isolate the obtained products. The present methodology proved to be quite suitable for scale-up and commercialization.

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