A two-step convenient sequence for the synthesis of previously inaccessible mono-Boc- protected bis-N-heterocyclic alkyl substituted ether derivatives 4 is described. Mitsunobu protocol was applied to the preparation of pyridinyl ether precursor 5. The reduction of the electron rich pyridinyl system 5 has been achieved catalytically using the combination of PtO2–H2SO4 or PtO2–pTsOH under a hydrogen atmosphere maintained by a gas balloon ...