Microwave‐Assisted One‐Step Synthesis of Palladium‐Encapsulated Covalent Organic Frameworks for Heterogeneous Catalysis

Abstract Metal‐encapsulated covalent organic frameworks (metal/COFs) represent an emerging paradigm in heterogeneous catalysis. However, the time‐intensive (usually 4 or more days) and tedious multi‐step synthesis of metal/COFs remains a significant stumbling block for their broad application. To address this challenge, we introduce a facile microwave‐assisted in situ metal encapsulation strategy to cooperatively combine COF formation and in situ palladium(II) encapsulation in one step. With this unprecedented approach, we synthesize a diverse range of palladium(II)‐encapsulated COFs (termed Mw‐Pd/COF) in the air within just an hour. Notably, this strategy is scalable for large‐scale production (~0.5 g). Leveraging the high crystallinity, porosity, and structural stability, one representative Mw‐Pd/COF exhibits remarkable activity, functional group tolerance, and recyclability for the Suzuki‐Miyaura coupling reaction at room temperature, surpassing most previously reported Pd(II)/COF catalysts with respect to catalytic performance, preparation time, and synthetic ease. This microwave‐assisted in situ metal encapsulation strategy opens a facile and rapid avenue to construct metal/COF hybrids, which hold enormous potential in a multitude of applications including heterogeneous catalysis, sensing, and energy storage.