The new ortho‐quinone quinoline 7‐(carboxymethoxy)‐3‐sulfoquinoline‐5,6‐dione was synthesized. The reaction of this quinoline‐5,6‐dione with hydroxylamine, hydrazine, phenylhydrazine, ethanol, semicarbazide, thiosemicarbazide, ethylenediamine, and benzene‐1,2‐diamine were studied. Ten new azaheterocyclic compounds were isolated and characterized by elemental analyses, IR, 1D NMR, 2D NMR, and MS spectra. Antioxidant activities of some obtained compounds were tested.