Abstract: A new iodine heterocyclic compound, 8-oxo-diquino(5, 6-b; 6′, 5′-e)-pyriodonium [Ⅲ] compound, white needles prims(m•p•221-2℃),was prepared in about 68% yield by treating 6,6′-diquinolyl oxide[Ⅱ] with iodosyl sulfate in concentrated sulfuric acid,following by pyridine [Ⅲ] The structures of [Ⅱ] and [Ⅲ] were confirmed by IR,~1HNMR, MS and elemental analysis.