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Nitration of N‐ethoxycarbonyl‐[U‐14C]aniline with two equivalents of nitric acid in sulfuric acid afforded N‐ethoxycarbonyl‐2,4‐dinitro‐[U‐14C]aniline which was deprotected quantitatively to 2,4‐dinitro‐[U‐14C]aniline. Selective hydrogenation provided 99.5% radiochemically pure [U‐14C]nitrophenylenediamine with specific activity 25.6 mCi/mmol in 20% radiochemical yield.