Conjugated hyperbranched polyphenylene nanoparticles are fabricated by cross coupling reactions between an A(2) type monomer 1,4-phenylenediboronic acid (1) and B-3 type monomers 1,3,5-triiodobenzene (2) and 1,3,5-tribromobenzene (3). The Suzuki-type polycondensation was conducted with a highly efficient heterogeneous catalyst to give conjugated polymeric nanoparticles which are soluble in a variety of organic solvents. The growth of the hyperbranched polyphenylenes are controlled and eventually terminated by the decomposition of the boronate terminal groups in basic aqueous media in the heterogeneous catalysis system. This method represents a new approach to produce soluble conjugated polymeric nanoparticles with simple and symmetrical monomers with more than two end groups (A(x) + B-y, x >= 2, y > 2). (C) 2015 Elsevier Ltd. All rights reserved.