Five new aza-crown ethers have been prepared by the condensation of 2,6-bis[(2-formylphenyl)oxymethyl] pyridine with different diamino compounds in hot methanol, the bis-Schiff bases without isolation were reduced with NaBH4 to afford the corresponding aza-crown ethers. The liquid membrane transport of alkali cations using the five new macrocycles as the ion-carriers was also studied. Five new aza-crown ethers have been prepared by the condensation of 2,6-bis [(2-formylphenyl) oxymethyl] pyridine with different diamino compounds in hot methanol, the bis-Schiff bases without isolation were reduced with NaBH4 to afford the corresponding aza-crown ethers. The liquid membrane transport of alkali cations using the five new macrocycles as the ion-carriers was also studied.