An efficient, direct and general synthesis of enantiopure γ-azido-tetrahydrofuran carboxylic acid monomers (
5–
8) from commercially available glycals, suitable to design peptidomimetic oligomers with predisposed conformation, is described. The single crystal X-ray study of
8 showed that the compound crystallized in orthorhombic space group. The crystal-packing showed the presence of weak intermolecular C–H
O and aliphatic C–H
π interactions.