3’,5’-Dimethoxy-4’-(2-vinyloxyethoxy)-4-nitrostilbene 2 and 3’,5’-dimethoxy-4’-(2-vinyloxyethoxy)-2,4-dinitrostilbene 5 were prepared by the reactions of 2-iodoethyl vinyl ether with 3’,5’-dimethoxy-4’-hydroxy-4-dinitrostilbene 1 and 3’,5’-dimethoxy-4’-hydroxy-2,4-dinitrostilbene 4, respectively. Monomers 2 and 5 were polymerized with cationic initiators to obtain polymers with the NLO-phores 3’,5’-dimethoxy-4’-oxy-4-nitostilbene and 3’,5’-dimethoxy-4’oxy-2,4-nitrostilbene in the side chain. The resulting polymer 3 and 6 were soluble in DMSO and DMF. The inherent viscosities of polymers were in the range of 0.28-0.33 dL/g in DMSO. Polymers 3 and 6 showed good thermal stabilities in their TGA thermograms, and the T-g values from DSC thermograms were in the range of 81-87 degrees C.