AbstractA series of homo‐oligomeric peptides derived fromγ‐benzyl‐L‐glutamate, Nps‐[L‐Glu‐(OBzl)]n+m−OBzl(4(n,m)) (n+m= 2 to 12, 15, 16, 18, 21, and 24), were synthesized for the first time by the DCC‐ONSu method using and activated easter. The identification and conformation of these peptides in cast films were investigated successfully by IR spectroscopy. It was found that the formation of the β‐structure begins with the tetrapeptide, and that of the α‐helix in the range from the hexapeptide to octapeptide. There is some evidence for small quantities of other conformational nuclei which may coexist as preferred conformations in peptides between the hexa‐ and decapetides. These effect cannot be attributed to sample purity since they could be sho