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In this study, a step‐by‐step method for the synthesis of platinum nanoparticles and copper(I) complex supported on mesoporous silica hollow spheres (Pt‐MSHSs‐Cu) is introduced. Scanning electron microscopy, transmission electron microscopy, powder X‐ray diffraction, Fourier transform infrared spectroscopy, nitrogen adsorption–desorption, energy‐dispersive X‐ray spectrometry, X‐ray photoelectron spectroscopy, and elemental and thermogravimetric analyses were applied for characterization of the surface, structure, size, phase composition, and morphology of the synthesized materials. The characterized material, Pt‐MSHSs‐Cu, was used as an efficient and heterogeneous catalyst in the Sonogashira coupling reaction under different reaction conditions. In comparison with MSHSs, Cu(I)‐functionalized MSHSs (MSHSs‐Cu), and Pt‐MSHSs samples, the Pt‐MSHSs‐Cu catalyst exhibited significantly increased catalytic performance with 91.50% yield. Therefore, the results obtained suggested a synergistic effect derived from platinum nanoparticles, MSHSs substrate, and copper(I) complex, which enhanced the rate of the Sonogashira coupling reaction.

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