Protected peptides containing an anti b-hydroxy tyrosine are synthesized in a straightforward and highly efficient manner through the direct and stereoselective addition of N-azidoacetyl-4-isopropyl-1,3-thiazolidine-2-thione to dialkyl acetals catalyzed by a nickel(II) complex, the forging of an amide bond by removal of the chiral auxiliary with an amino ester, and final coupling with a third amino acid.