A hexapeptide containing a fl-D-Galp-(1 ~ 3)-a-D-GalpNAc-(1 ~ O)-L-threonine unit was synthesized using glycosylated pentafluorophenyl esters in an Fmoc-based strategy. In all of the glycosylation reactions, trichloroacetimidates were successfully employed. The disaccharide moiety was prepared from tetra-O-acetyl-c~-o-galactopyranosyl trichloroacetimidate and tert-butyldimethylsilyl 2-azido-6-O-benzoyl-2-deoxy-/3-E-galactopyranoside with boron trifluoride etherate as a catalyst. The glycosylated active esters were obtained in the reaction of a and /3 2,3,4,6-tetra-O-acetyl-/3-o-galactopyranosyl-(1 -~ 3)-4-O-acetyl-2-azido-6-O-benzoyl-2-deoxy-D-galactopyranosyl trichloroacetimidates with Fmoc-protected pentafluorophenyl esters of L-serine and L-threonine in the presence of trimethylsilyl trifluoromethanesulfonate as Lewis acid. The glycosylated pentafluorophenyl ester of L-threonine was transformed into glycopeptides via a solid-phase synthesis. Azide reduction and N-acetylation were performed on the solid phase with a thioacetic acid-pyridine mixture. The glycopeptide was then cleaved from the resin with strong acid, also removing the acid-labile protecting groups of the peptide chain. Finally, the acyl groups used for sugar protection were cleaved with sodium methoxide, affording the completely deprotected N-acetyl-L-leucyl-L-glutamyl-O-[/3-D-galactopyranosyl-(1 ~ 3)-2-acetamido-2-deoxy-a-ogalactopyranosyl]-L-threonyl-L-seryl-L-threonyl-glycinamide (1) in high purity.