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Synthesis of the C‐ and N‐terminally deprotected monocyclic tryptathionine peptide 5: a) Boc2O, NaHCO3, dioxane/H2O, r.t., 16 h, 99 %; b) SO2Cl2, CHCl3, r.t., 1 h; c) 8, NaHCO3, CHCl3, 0 °C to r.t., quant., d) H‐Gly‐Ile‐Gly‐OH, CO(OSu)2, collidine, acetonitrile/H2O, r.t., 2 h; e) PTSA, THF, r.t., 2 h, 70 % over 2 steps; f) T3P, DIPEA, DMF, r.t., 16 h, 70 %, g) TFA/H2O (7:3), r.t., 2 h, quant.
