Oxidative coupling of 2-hydrazino-4,6-disubstituted 1,3,5-triazines with N,N-disubstituted anilines was studied. The oxidative coupling reaction proceeded by the use of potassium hexacyanoferrate(III) as the oxidizing agent in aqueous acetic acid solution buffered at pH 4.4 with sodium acetate at room temperature to give corresponding phenylazo-1,3,5-triazines in good yields.