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[14C]Azodicarbonamide, a potent inhibitor of HIV‐1 and HIV‐2 was prepared by reaction of hydrazine sulfate with potassium [14C]cyanate, followed by oxidation of the resulting biurea. The overall radiochemical yield was 57% and the specific activity of the product was 1.48 GBq/mmol (39.9 mCi/mmol).