(1-Pyrenyl)butadiyne derivatives 5 and 6 with a methylene chain and a L-alanine moiety as a chiral group were synthesized, and the end group of 5 and 6 was ethyl ester and carboxylic acid, respectively. These compounds could be polymerized in the crystals by UV irradiation at 365nm. The regular solid-state polymerization was confirmed for 5 although 6 showed irregular polymerization. Their nanoaggregate water dispersions were obtained by the reprecipitation method. Morphology of their nanoaggregates was studied by SEM, and helical nanoribbons and circle domains were observed for 5 and 6, respectively.