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This paper describes synthesis of Pd-containing catalysts of Suzuki cross-coupling based on aminofunctionalized hypercrosslinked polystyrene. The investigation of the influence of a palladium concentration, solvent composition, temperature, type and concentration of base, and a type of a gas phase was carried out. It was shown that the catalyst developed allows achieving conversion of 4-bromoanisole higher than 98% for less than 1 h at mild reaction conditions and in the absence of a phase transfer agent. Catalyst reduction was found to result in formation of small Pd nanoparticles (about 3 nm in diameter) and a large number of Pd clusters, which are highly active in Suzuki-Miyaura cross-coupling (conversion of 4-bromoanisole reached 90.2% for 3 h).

The influence of the content of a hydrophilic Pd(II) compound (disodium tetrachloropalladate, Na 2 PdCl 4 ) on its adsorption and nanoparticle (NP) formation in the pores of hydrophobic micro/mesoporous hypercrosslinked polystyrene (HPS) was systematically investigated. The morphology and composition of HPS-Pd nanocomposites were studied using transmission electron microscopy, X-ray fluorescence measurements, and liquid nitrogen physisorption. The size of Pd-containing NP was found to depend on the content of the hydrophilic Pd(II) compound. Catalytic testing of these nanocomposites in the partial hydrogenation of acetylene alcohols was carried out to illustrate the influence of the NP size on the catalytic activity. The highest catalytic activity was achieved for HPS/Pd-0.1 %, forming small NP.