Poly[1-(2-methoxyphenyl)penta-1,3-diyn-5-ol] [(1,2)-PMDO] was prepared by NbCl5/(n-Bu)(4)Sn catalyzed metathesis of (1,2)MDO followed by spin-casting in methylene chloride. Thin films of resulting polymers were pyrolyzed at various temperatures. UV, IR, and Raman spectroscopic studies were carried out to determine the chemical structure of the films during pyrolysis. The electrical conductivity of the films could be varied on cabonization at different temperatures.