Unsymmetrically bis(chlorobenzoylated) 2,2'-dimethoxybiphenyl (7) has been successfully prepared via 4-chlorobenzoylation of 2-bromoanisole, Suzuki coupling of the resulting benzophenone, and 3-chlorobenzoylation of the coupling product. Nickel complex-mediated aromatic coupling polymerization of the obtained unsymmetrically bis(chlorobenzoylated) monomer (7) readily affords the wholly aromatic polyketone having a sufficiently high molecular weight and good solubility in organic solvent, such as chloroform. The alignment of the polyketone (6) is disclosed to be random on the basis of the H-1 NMR spectrum. (C) 2004 Elsevier B.V. All rights reserved.