Three new
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,
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′-diimine ligands were synthesized based on condensation of 1,10-phenanthroline-5,6-dione with 1,2-phenylenediamine derivatives using different approaches. All compounds were fully characterized by IR,
1H and
13C NMR, UV–visible, and MS spectroscopies. We report the first example of a dipyrido[3,2-
f:2′,3′-
h]quinoxalino[2,3-
b]quinoxaline, which exhibits a strong absorption at 430 nm and an interesting electrochemical behavior. These new molecules may have biological potential and are of synthetic and technological importance.