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Two 3D-hybrid monolithic catalysts containing immobilized copper and palladium species on a silica support were synthesized by 3D printing and a subsequent surface functionalization protocol. The resulting 3D monoliths provided a structure with pore sizes around 300 μm, high mechanical strength, and easy catalyst recyclability. The devices were designed to perform heterogeneous multicatalytic multicomponent reactions (MMCRs) based on a copper alkyne–azide cycloaddition (CuAAC) + palladium catalyzed cross-coupling (PCCC) strategy, which allowed the rapid assembly of variously substituted 1,2,3-triazoles using a mixture of tBuOH/H2O as solvent. The reusable multicatalytic system developed in this work is an example of a practical miniaturized and compartmental heterogeneous 3D-printed metal catalyst to perform MMCRs for solution chemistry.

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