1,1’-Dialkylferrocene-3,3’-dicarbaldehydes (1a-c) with long alkyl chains such as ethyl, hexyl, and dodecyl groups were prepared in 13-25% yield via three-step reactions. The titanium-induced dicarbonyl-coupling reaction of 1a-c gave poly(1,1’-dialkyl-3,3’-ferrocenylenevinylene)s (2a-c) in quantitative yields, which were the molecular weights of 3000-10,000 and highly soluble in chloroform, benzene, and hexane. The electrical conductivity and the third-order nonlinear optical susceptibility for poly(1,1’-dihexyl-3,3’-ferrocenylenevinylene) (2b) were estimated to be 1 X 10(-2) S/cm on doping with iodine and 1-4 X 10(-12) esu at a wavelength of 1-2.4 mu m, respectively.