Jad Yahya E, Khattab Sherine N, de la Torre Beatriz G, Govender Thavendran, Kruger Hendrik G, El-Faham Ayman, Albericio Fernando
Catalysis and Peptide Research Unit, School of Health Sciences, University of Kwazulu-Natal, Durban 4001, South Africa.
Org Biomol Chem. 2014 Nov 14;12(42):8379-85. doi: 10.1039/c4ob01612b.
Peptide-bond formation is a key process in the synthesis of peptide oligomers. Among the many coupling techniques reported, carbodiimides combine strong acylation potency and smooth reaction conditions and are commonly used in the presence of additives. Recently, ethyl 2-cyano-2-(hydroxyimino)acetate (OxymaPure) has emerged as a highly reactive alternative to the classic and explosion-prone benzotriazolic additives, namely 1-hydroxybenzotriazole (HOBt) and 1-hydroxy-7-azabenzotriazole (HOAt). Here we report on a new oxime additive 5-(hydroxyimino)-1,3-dimethylpyrimidine-2,4,6(1H,3H,5H)-trione (Oxyma-B). This new additive showed satisfactory solubility in various solvents (DMF, ACN, and THF). It was also more effective in the control of optical purity during the synthesis of Z-Phg-Pro-NH2, Z-Phe-Val-Pro-NH2, H-Gly-Ser-Phe-NH2, H-Gly-Cys-Phe-NH2, H-Gly-Cys(Acm)-Phe-NH2 and H-Gly-His-Phe-NH2 than related Oxyma- and benzotriazole-based reagents. Oxyma-B also proved to be advantageous compared to the related HONM, because the latter cannot be used with the carbodiimide. Furthermore, Oxyma-B showed satisfactory performance in assembling demanding sequences such as the Aib-enkephalin pentapeptide (H-Tyr-Aib-Aib-Phe-Leu-NH2).
肽键形成是肽低聚物合成中的关键过程。在众多已报道的偶联技术中,碳二亚胺具有强大的酰化能力且反应条件温和,通常在添加剂存在的情况下使用。最近,2-氰基-2-(羟基亚氨基)乙酸乙酯(OxymaPure)已成为经典且易爆炸的苯并三唑类添加剂(即1-羟基苯并三唑(HOBt)和1-羟基-7-氮杂苯并三唑(HOAt))的高反应性替代品。在此,我们报道一种新的肟添加剂5-(羟基亚氨基)-1,3-二甲基嘧啶-2,4,6(1H,3H,5H)-三酮(Oxyma-B)。这种新添加剂在各种溶剂(N,N-二甲基甲酰胺、乙腈和四氢呋喃)中表现出令人满意的溶解性。在Z-Phg-Pro-NH2、Z-Phe-Val-Pro-NH2、H-Gly-Ser-Phe-NH2、H-Gly-Cys-Phe-NH2、H-Gly-Cys(Acm)-Phe-NH2和H-Gly-His-Phe-NH2的合成过程中,它在控制光学纯度方面也比相关的基于Oxyma和苯并三唑的试剂更有效。与相关的HONM相比(后者不能与碳二亚胺一起使用),Oxyma-B也被证明具有优势。此外,Oxyma-B在组装要求较高的序列(如Aib-脑啡肽五肽(H-Tyr-Aib-Aib-Phe-Leu-NH2))时表现出令人满意的性能。