Poly(1,4-phenylenevinylene) derivative, 58-poly(NO2STMPV-co-IMPV), consisting of poly[2-methoxy-5-{3-(4-nitrostilben-4’-yl-oxy)propoxy}phenylenevinylene] (poly(NO2STMPV)) and poly(2-isopropoxy-5-methoxy-1,4-phenylenevinylene) (poly(IMPV)) was synthesized through the Wessling’s precursor method. Films of the precursor copolymers were eliminated either by way of thermal treatment or using strong acidic conditions. The electrical conductivities of FeCl3-doped 58-poly(NO2STMPV-co-IMPV) were found to be between 10(-1)-10(-4) S/cm. The second-order nonlinear optical susceptibility (d(33)) of this copolymer was about 2.0 pm/V.