As part of our current investigations of nitropyridines, we hereby report the preparation of a new annulated heterocycle by C‐azo coupling. Thus, the azacinnoline, pyrido[3,4‐c]pyridazin‐4(1H)‐one (38%), was prepared from 4‐acetyl‐3‐aminopyridine via diazotization. 1H, 13C, and 15N NMR spectroscopic investigations revealed that the azacinnoline exclusively exists in the NH‐keto tautomeric form in DMSO‐d6, CD3OD, and D2O. J. Heterocyclic Chem., (2011).