The syntheses of two sulfated pentasaccharides: β-d-Gal6SO3Na-(1→ 3)-[β-d-Gal-(1→ 4)-α- l-Fuc-(1→ 3)-β-d-GlcNAc-(1→ 6)]-α-d-GalNAc→ OMe (1) and β-d-Gal6SO3Na-(1→ 3)-[β-d- Gal-(1→ 4)-α-l-Fuc-(1→ 3)-β-d-GlcNAc6SO3Na-(1→ 6)]-α-d-GalNAc→ OMe (2) by using LewisX trisaccharides 12 and 16 as glycosyl donors are described. Sulfated oligosaccharides 1–2 and intermediate compounds are fully characterized by 2D 1H–1H ...