A new diamide N,N,N′,N′-tetrahexylmalonamide (THMA) was synthesized, characterized and used in the extraction of U(VI) from nitric acid solutions. N,N,N′,N′-tetrabutylmalonamide (TBMA) was also studied to test the steric hindrance. Factors affecting this extraction system, the concentration of the extractant, aqueous nitric acid and NaNO3 and the temperature were investigated. The IR spectral study was also made of the extracted species.