Oxidation of bis‐2,4‐pyrimidinylhydrazones of various araldehydes with two equivalents of iodobenzene diacetate in dichloromethane provides an efficient and easy method for the synthesis of eight new 3,9‐diaryl‐bis‐1,2,4‐triazolo[4,3‐a][4,3‐c]pyrimidines. © 2006 Wiley Periodicals, Inc. Heteroatom Chem 17:653–655, 2006; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.20250