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The method uses synthesis of Boc\u2010didepsipeptides by reaction of free hydroxy acids with Boc\u2010amino acid <jats:italic>N<\/jats:italic>\u2010hydroxysuccinimide esters catalyzed by 4\u2010dimethylaminopyridine and chain elongation of the free depsipeptides by the reaction with Boc\u2010amino acid <jats:italic>N<\/jats:italic>\u2010hydroxysuccinimide esters in an organic solvent system of acetonitrile\u2010tetrahydrofuran. The Boc\u2010depsipeptide free acids were activated as their <jats:italic>N<\/jats:italic>\u2010hydroxysuccinimide esters, which were polymerized after removal of the Boc\u2010protecting group. \u00a9 2004 Wiley Periodicals, Inc. 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