Pd‐catalyzed Suzuki–Miyaura cross‐coupling (SMC) reactions are important in chemistry. In this work, using electrospinning technology, we prepared a novel type of composite catalyst with ligand structures such as urea‐Pd/PAN (polyacrylonitrile) and used them to catalyze SMC reactions in nontoxic systems and “green” conditions (air atmosphere, low temperature, and short reaction time). This method of preparing hybrid materials is simple and easy to operate. The higher catalytic activity of the catalysts is attributed to active centers with rich electrons transferred from ligands with unique structures, which can decrease the activation energy of the rate‐determining step (oxidative addition). In addition, urea‐Pd/PAN composite catalysts exhibit higher catalytic performance than those reduced by H2 because of the smaller size of active species and the more‐efficient oxidative addition to Pd0–ligand complexes compared to Pd0.

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