Orthogonally protected thioamide-containing dipeptides were efficiently and cleanly prepared from the precursor dipeptides using Curphey’s method (P₄S₁₀, hexamethyldisiloxane (HMDO), reflux, DCM) in 67–96% isolated yield. This was in contrast to the use of Lawesson’s or Berzelius’ reagents where significant issues with reaction non-completion, decomposition and purification were observed. Subsequent clean removal of the dipeptides’ t-butyl ester protecting groups gave thioamide dipeptide acids which were suitable for use in solid-phase peptide synthesis (SPPS).

中文翻译：

---

用于固相肽合成的正交保护的硫酰胺二肽的合成

使用Curphey方法（P ₄ S ₁₀，六甲基二硅氧烷（HMDO），回流，DCM）从前体二肽中高效，清洁地制备了受正交保护的含硫酰胺的二肽，分离产率为67-96％。这与使用Lawesson试剂或Berzelius试剂相反，后者在反应不完全，分解和纯化方面存在重大问题。随后干净地除去二肽的叔丁酯保护基，得到适合用于固相肽合成（SPPS）的硫代酰胺二肽酸。