A novel poly(1,4-phenylenevinylene) (PPV) derivative containing an azobenzene side chain was prepared via a dehydrochlorination ro ute. Poly{2-methoxy-5-[(4-(4-methoxyphenylazo)phenyloxy)hexyloxy]-1,4-phenyle nevinylene}, which is soluble in ordinary solvents such as chloroform, tetrahydrofuran (THF), acetone, xylene, etc., was characterized by FTIR,H-1 NMR, GPC, and W-visible spectroscopies, thermogravimetric analysis (TGA), and cyclic voltammetry. The photoluminescence spectrum of the polymer showed an emission maximum at lambda = 550 nm.