This experiment describes the reaction of palladium(II) chloride with 1,5-bis(diphenylphosphino)pentane by grinding the two powders together in the solid state. The product is the precursor for the metalation reaction at one of the methylene carbon atoms of the ligand's backbone. The final product is known to be a catalyst for Suzuki-Miyaura coupling. Interesting NMR spectra combine with the example of a mechanical synthesis and a reflux under nitrogen to make this a useful upper-level undergraduate inorganic experiment. (Contains 1 figure and 1 scheme.)