AbstractMetal nanoparticles immobilized in the confined space are a catalogue of efficient and widely used catalysts. Herein we develop a gel‐based bimetallic nanoparticle catalytic system with different ratios of Pd/Cu NPs by wet impregnation and reduction using a stable covalent gel (triazole‐A1B1) as a porous support. Triazole‐A1B1 gel is synthesized from 1,4‐diazidobenzene (A1) and tetrakis(4‐ethynylphenyl)methane (B1) via Cu(I)‐catalyzed azide‐alkyne clcloaddition. The bimetallic Pd/Cu metal nanoparticles are highly dispersed and uniformly distributed with an average particle size distribution of 2.06–3.29 nm. Cu/Pd@A1B1 shows high catalytic efficiency in catalyzing Sonogashira‐Hagihara and Mizoroki‐Heck coupling reactions. The introduction of oxygenophilic Cu effectively improves the catalytic activity of the system. In addition, Cu1Pd2@A1B1 shows good reusability. Especially, it can be reused five times and maintains high catalytic activity without significant deactivation in Mizoroki‐Heck coupling reaction.

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