thylformamide (DMF) afforded the desired glycopentapeptide allyl ester 9, whose structure was likewise confirmed by elemental analysis and spectroscopic data (I3C-NMR: 6= 102.9, C-1, Jp)c-H)= 163 Hz (dimethyl sulfoxide)).The allyl group has thus proven to be a valuable achiral carboxy-protecting group even for difficult peptide and glycopeptide syntheses, and can be used in conjunction with N-terminal Z -and Boc-protecting groups. Also noteworthy is that the four glycopeptide allyl esters 3a, 38, 6 and 9 are crystalline.