Sustainable Synthesis of Palladium‐Immobilized Covalent Organic Frameworks: A One‐step Sonochemical Strategy

Abstract The rapid and environmentally benign synthesis of metal‐immobilized covalent organic frameworks (metal/COFs) for heterogeneous catalysis is a pervasive challenge, as the mainstream synthesis is exceedingly time‐consuming (up to four days) and demands the use of hazardous solvents. Herein, we describe a sustainable and efficient one‐step sonochemical strategy for constructing diverse palladium (II)‐immobilized COFs (Pd(II)/COFs). By merging the sonochemistry‐assisted COF synthesis and in situ Pd (II) immobilization into a single step, this strategy enables the rapid formation of Pd(II)/COF hybrids within an hour under ambient conditions using water as the solvent. Notably, gram‐scale synthesis of Pd(II)/COFs is achievable. The resulting Pd(II)/COFs exhibit superb crystallinity and high surface area, leading to remarkable activity, excellent functionality tolerance, and high recyclability for the Suzuki–Miyaura cross‐coupling reaction of aryl bromides and arylboronic acids at room temperature. This one‐step sonochemical strategy effectively addresses the long‐lasting limitations of traditional multistep synthesis, paving a fast and sustainable avenue to diversified metal/COF hybrids for heterogeneous catalysis and potentially other applications.