N-Acyl-1,3-diaryl-2-azaphenalene derivatives have been synthesized by one-pot condensation reaction of aromatic aldehydes, 2,7-naphthalenediol, carboxylic acids, and aqueous ammonia (25 %). Different aromatic aldehydes and carboxylic acids have been used in the reaction and the products were always obtained in good to high yields. The method is simple, solvent free, and involves a short reaction time. These relatively rapid reactions possibly proceed via a Betti reaction mechanism.