A redox-active molecule, 2,5,8-tri(4-pyridyl)-1,3-diazaphenalene (TPDAP), was synthesized by four-step reactions. The two-step redox reaction was revealed by solid-state cyclic voltammetry. The crystal was obtained by sublimation under reduced pressure and characterized by single-crystal X-ray structure determination. Oxidation of TPDAP produced a neutral radical that was characterized by ESR.