A solid-phase-Fmoc-based-synthesis strategy is described for oligourea peptidomimetics as well as a convenient general synthesis approach for the preparation of the required building blocks 5a-j and 5k. These are suitable for use in peptide or robot synthesizers, which is illustrated by the synthesis of oligourea peptidomimetics of part of Leu-enkephalin (10) and a neurotensin derivative (17).

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A procedure for the solid‐phase synthesis of oligourea peptidomimetics starting from Boc‐protected monomers is described. The compounds are prepared on Tentagel® resin and can be obtained selectively either as the C‐terminal free acids with UV irradiation when a photocleavable linker is used or as C‐terminal hydantoins with 10% TEA/MeOH and a catalytic amount of KCN.