Through free‐radical trapping experiments we have established, for the first time, the combination of arylhydrazines with o‐iodoxybenzoic acid (IBX) for the generation of aryl free radicals. On the basis of this finding, a method was developed for the N‐arylation of aromatic amines under mild conditions (base‐free, –5 °C) by using arylhydrazines as the arylating counterpart and arylamines. The scope of this method was demonstrated by using a number of arylhydrazines and arylamines, which gave the N‐arylated amines in good yields.

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Formation of the nitrile was the outcome of the investigation of biochemically significant oxidative decarboxylation of amino acids using o-iodoxybenzoic acid (IBX) in aqueous ammonia system.

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Biologically important process of oxidation of amidoximes has been investigated using IBX (oiodoxybenzoic acid) and combination of IBX with TEAB (tetraethylammonium bromide). The reaction proceeds with high % conversion leading to selective formation of amide and nitrile depending upon the combination of reagents.