The oxidative coupling polymerization of 2,3-dihydroxynaphthalene with the novel dinuclear-type copper(H) catalysts successfully produced poly(2,3-dihydroxy-1,4-naphthylene). For example, the MeOH-insoluble polymer with a number average molecular weight of 4.4 xs 10(3) from the polymerization using the complex Of CuCl2 and N,N'-bis(2-morpholinoethyl)-p-xylylenediamine (p-1) at room temperature under an O2 atmosphere followed by acetylation of the hydroxyl groups was obtained in 63% yield. The structures of the tetraamine ligands and the counter anion of the copper(II) salts significantly influenced the catalyst activity. The polymerization of 2,2'-dimethoxy-1,1'-binaphthalene-3,3'-diol with the 2CuCl(2)-p-1 catalyst, however, resulted in a lower yield. (c) 2005 Wiley Periodicals, Inc.