Keywords: Acetylene / Heterocycles / X-ray absorption spectroscopy / UV/Vis spectroscopy / Fluorescence spectroscopy (10), and 2,6-dimethyl-3-(pyrrol-2-yl)-5-[2-(1-vinylpyrrol-2-yl)]pyridine (11) have been synthesized from the oximes of the corresponding diacetylpyridines in a one-pot procedure by treatment with acetylene in MOH/DMSO systems (M = Li, K) at 80-140°C under pressures of 25-30 atm, thus illustrating the applicability and general character of the reaction for synthesis of diverse dipyrrole-pyridine assemblies and their N-vinyl and acetyl derivatives. A stable 4·DMSO
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