Abstract: The synthesis of β-casomorphin H-Tyr-Pro-Phe-Pro-Gly-OH employing Boc group for N α-protection and 9-fluorenylmethyl chloroformate (Fmoc-CI) for the formation of peptide bond is described. The protocol employing Fmoc-Cl as coupling reagent is found to be simple, efficient and rapid. All the intermediate peptides as well as the final protected peptide Boc-Tyr (t Bu)-Pro-Phe-Pro-Gly-OMe have been isolated and fully characterized. ...