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A new polythiophene derivative bearing an azobenzene substituent at the end of a ethylenic side‐chain was synthesized and characterized by FT‐IR spectroscopy, 1H and 13C NMR spectroscopy, DSC, TGA, XRD, and UV‐vis spectroscopy. Its electrical conductivity was measured and its second‐order NLO activity was by SHG. Structure‐property relations were elucidated by comparison with a similar polymer only partially substituted by the NLO‐active chromophore. The molecular design of the chromophoric system allows high and stable non‐linear coefficients d33 to be obtained, making these polymers suitable for the construction of second‐harmonic generators with improved efficiency and life‐time.

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