An efficient procedure was developed for the removal of methyl groups from aryl methyl ethers, without racemization, in derivatives of unusual amino acids that are of significant importance in the design of highly selective peptide protein ligands with specicific conformational topographical features. Demethylation of aromatic amino acids can result in an appreciable increase in receptor affinity, hence the new mild procedure which have been developed represents a facile practical method for demethylation of Tyr (OMe) derivatives, including novel sidechain ring or C-3 modified analogs.