A sample of cyclic oligo(undecanamide)s (nylon 11s), containing from the cyclic monomer to at least the cyclic hexamer, was conveniently prepared (57% yield) by the cyclo-oligomerization of 11-aminoundecanoic acid p-nitrophenyl ester under high dilution conditions.The cyclics, obtained free of linear oligomers by virtue of their greater solubilities in chloroform, were analyzed by fast atom bombardment mass spectrometry (FABMS), high pressure liquid chromatog. (HPLC), gel permeation chromatog. (GPC) and 1H NMR spectroscopy.The latter, which displayed a series of N-H signals reflecting the proportions of the various cyclics, was the most convenient method for analyzing the cyclic oligo(undecanamide)s.A sample of cyclic alternating oligo(undecanamide-undecanoate)s, containing from the cyclic monomer to at least the cyclic undecamer, was conveniently prepared (57% yield) from (11-aminoundecanoyl)-11-oxyundecanoic acid p-nitrophenyl ester in a similar manner.Linear oligo(undecanamide-undecanoate)s were prepared from the appropriate ω-bromo acid using a phase transfer catalyzed reaction.These cyclic and linear oligomers, which were much more soluble than the corresponding oligo(undecanamide)s, were analyzed by FABMS, GPC, and 1H NMR spectroscopy.For these oligomers GPC was the most convenient method of anal.