A convenient, one-pot method for the synthesis of diazonium salt has been developed by the sequential diazotization of aromatic amines with NaNO2, polymer- supported periodic acid (PPIA) and 2-naphthole under solvent-free conditions at room temperature. By using this method, several types of aromatic amine, containing electron-withdrawing and electron-donating groups, were rapidly converted to the corresponding azo dyes in good to excellent yields. The ensuing aryl diazonium salts supported on polymer (aryl diazonium polymer), ArN2 +IO4 - were sufficiently stable to be kept at room temperature in the dry state. The use of mild reaction conditions and an inexpensive procedure are further advantages of this method. Manuscript profile