The synthesis and structural analysis of glucosamide surfactants of the general formula C n H 2n+1 NH(CH 2 ) 6 NHCO(CHOH) 4 CH 2 OH (n = 8, 10, 12) were described, and the surface activity properties of the surfactants were studied, and the interfacial tensions between n -octane and the aqueous surfactant solution were measured. N -alkylhexanediamines were synthesized by the alkylation of the 1,6-hexanediamine with alkyl bromide. The glucosamide surfactants, N -alkyl- N ′-glucosylhexanediamine (C n GA), were prepared by amidation of the precursor diamine with D-gluconic acid δ-lactone. They were structurally characterized by IR, 1 H NMR and MS. They reduced the surface tension of water to approximately 28–33 mN · m −1 at concentration levels of (0.2–1.0) × 10 −3 mol · L −1 , and reduced the interfacial tensions between n -octane and the aqueous surfactant solution to approximately 1–2 mN · m −1 at concentration levels of (0.3–4.2) × 10 −3 mol · L −1 .