The synthesis of [2, leucine-enkephalin by the catalytic tritiation of [2,6-dibromo-Tyr'] leucine-enkephalin is described. The precursor amino acid, 2,6-dibromo-~~-tyrosine, was synthesized in three steps from 2,6-di bromo-4-methoxytoluene. The protected [ 2,6-di bromo-Tyrl] leucine-enkephalin derivative was prepared by solid-phase synthesis, followed by epimeric resolution on H PLC. The peptide was tritiated catalytically to yield [3H -Tyrl] leucine-enkephalin with a specific radioactivity of 1.37 TBq/mmol. The distribution of tritium was investigated by H PLC with radioisotope detection following enzymatic hydrolysis, and confirmed that the tritium label was entirely located at the tyrosine residue.