Abstract Utilizing N??benzyloxycarbonyl??(1a) and N??tert??butoxycarbonyl??(S)??glutamine (1b), a highly efficient and practical method for the synthesis of N 2??benzyloxycarbonyl??and N 2?? tert??butoxycarbonyl??(S)??2, 4??diaminobutanoic acids (2a and 2b) has been developed. Reaction of (S)??glutamine derivatives with iodosobenzene diacetate in a mixture of THF?? water at 4° C afforded selectively protected (S)??2, 4??diaminobutanoic acids in good yields.