Even in the case of a challenging Gly leading to a primary radical, macrocycle 13e could still be isolated in 17% yield. When lower yield was obtained for the macrocyclization, iodoalkynes and solvent adducts were observed as additional side products (See the Supplementary Information for details). Considering the importance of N-methylated residue for improving membrane permeability and hydrophobicity in drug discovery, peptide-EBX 3e containing N-methyl Val was also examined and it afforded cyclic peptide 13f in 37% isolated yield as two separable diastereoisomers.