Background: Nitriles are industrially important intermediates for the production of agrochemicals, pharmaceuticals, polymers, dyes, and pigments.[1] In addition, they serve as potential synthon for the functional group transformation and heterocyclic synthesis.[2] The use of various catalytic systems has been established for the oxidative transformation of nitrile from the substrates like alcohols, amines and amides.[3] The direct oxidative rearrangement of alkene,[4] and methyl arenes,[5] into nitriles have also been known. Methods: Ferric hydrogen sulfate was prepared and conducted to find the advantage of it in the conversion of aldehydic compounds into nitrile-containing ones. We have chosen 4-chlorobenzaldehyde as our model compound for the desired transformation. Therefore, the reaction conditions were initially optimized using the mole-ratio of the catalyst, reaction time, temperature of the reaction, the kind of solvent for the model reaction. After the optimization, the treatment of various derivatives of aldehydic-containing compounds with hydroxylamine hydrochloride in the presence of catalytic amount of Fe(HSO 4 ) as catalyst in refluxing DMF gave the corresponding nitrile compounds in good to excellent yields. 3

Keywords