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As a consequence of the organogel formation, we explored the possibility to run a light\u2010induced topochemical polymerization. This is a typical reaction of ordered diacetylene moieties taking advantage from their organized packing mode resulting from fiber formation. Evidence for the generation of peptide\u2010based polydiacetylenes is provided by Raman, UV\u2013Vis, and CD spectroscopies and a set of microscopic techniques. Finally, we succeeded in processing a polymeric composite by use of the electrospinning technique, starting from a mixture of a dipeptide\u2010based diacetylene and polymethyl methacrylate. 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