Abstract: | Novel fully π‐conjugated poly(arylene ethynylene)s 1 and 2 having diphenylmaleimides in the backbone were prepared utilizing a Pd(0)‐Cu(I) catalyzed coupling reaction (Sonogashira method) of N‐alkyl substituted 1,2‐di(4‐bromophenyl) maleimides ( 5 and 6 ) with 1,4‐diethynylbenzene. Whereas polymer 1 with an N‐hexyl side chain showed low solubility, 2 having an N‐ dodecyl group was completely soluble in common organic solvents. Determined by GPC, M̄w of 2 was 45 800 Da with a polydispersity index of 2.5. Polymer 2 showed UV‐visible absorption maxima at 330 nm and 413 nm and greenish yellow fluorescence with a maximum of 530 nm. |