The Rh(III)-catalyzed regioselective C(sp2)-H bond functionalization represents a facile tool for synthesizing valuable organic molecules precisely. However, in the face of pharmaceutical applications, challenges such as cost, reusability, and metal residue issues are always encountered under homogeneous reaction conditions. Herein, we report a synthesis of Rh(III)-covalent organic framework (RhCOF-SYNU-1) for heterogeneous regioselective C(sp2)-H bond functionalization. The suitable post-modification and metal immobilization endows RhCOF-SYNU-1 with multiple characteristics, including the adaptable and homo-dispersed Rh(III) centers, the extended conjugation system, and considerable stability. Hence, RhCOF-SYNU-1, serving as an all-in-one catalyst by integrating the roles of transition-metal catalyst, photocatalyst, and metal-center ligand, demonstrates excellent catalytic performance in various visible-light-driven or thermal regioselective C(sp2)-H bond functionalization reactions. Notably, the inherent robustness of RhCOF-SYNU-1 ensures its long-term use and simultaneous recycling with Cu oxidant under sophisticated organic reaction conditions, constituting a beneficial strategy for sustainable Rh(III) catalysis.
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