A green experiment is described here for direct fabrication of carboxymethylcellulose-supported palladium nanoparticles (PdNPs@CMC) in situ through a simple self-assemble and self-reduction process between carboxymethylcellulose (CMC-Na) and PdCl2 solution. The PdNPs@CMC was well characterized by ICP, UV-Vis, XPS, FTIR, SEM, and TEM techniques. The in situ synthesized PdNPs@CMC was proved to be an efficient catalyst for Suzuki-Miyaura coupling reaction under mild aerobic conditions. The superior catalytic performance of PdNPs@CMC is attributed to the coordination with carboxyl groups (−COO−) and free hydroxyl groups (−OH) as well as polymeric capping effect of CMC. Moreover, the catalyst showed no significant loss of its activity at least three consecutive cycles. This laboratory class is involved in the preparation and characterization of PdNPs@CMC as well as its catalytic application in Suzuki−Miyaura cross coupling reaction under green conditions. This laboratory class is suggested to divide into two parts. The first part includes the fabrication of catalyst in situ through a self-assemble and self-reduction of Pd(II) with CMC−Na, and characterization of the as-prepared catalyst using various techniques. The second part employs the resulting catalyst to perform a microscale Suzuki-Miyaura reaction, recycling of catalyst, and characterization of the product. By design, this comprehensive experiment set up for the third-year undergraduate, and aim to make students comprehend the concept of ion-exchange reaction, reduction reaction, carbon-carbon coupling reaction, supported catalysts, nanoparticles, and green chemistry as well as train the fundamental operation capability of students, and improve their experimental skills. 
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