A very easy sequential metathesis for the synthesis of Pd(II)-CMC@Ce(OH)4 organic/inorganic hybrid and its application as effective pre-catalyst for the Suzuki-Miyaura reaction have been reported. It was found that the Pd nanoparticles (Pd NPs) were formed in situ in the course of the Suzuki-Miyaura couplings when Pd(II)-CMC@Ce(OH)4 was used as a pre-catalyst. The activity of the Pd NPs in the reaction was enhanced synergistically by the unique redox properties (Ce3+/Ce4+) of Ce(OH)4 and coordination with carboxyl groups as well as free hydroxyl groups of the hybrid of CMC@Ce(OH)4. The results exhibit the Pd(0)-CMC@Ce(OH)4 is super over Pd(II)@CMC, Pd(II)@CeO2, and Pd(II)@Ce(OH)4 catalysts in the Suzuki-Miyaura reaction. Moreover, the catalyst could be easily separated by simple filtration and reused at least seven runs without losing its activity.
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