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Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis

The suppression of side reactions is one of the most important objectives in peptide synthesis, where highly reactive compounds are involved. Recently, the violuric acid derivative Oxyma-B was introduced into peptide synthesis protocols as a promising additive to efficiently control the optical puri...

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Detalles Bibliográficos
Autores principales: Orlandin, Andrea, Guryanov, Ivan, Ferrazzano, Lucia, Biondi, Barbara, Biscaglia, Francesca, Storti, Claudia, Rancan, Marzio, Formaggio, Fernando, Ricci, Antonio, Cabri, Walter
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2022
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9268172/
https://www.ncbi.nlm.nih.gov/pubmed/35807480
http://dx.doi.org/10.3390/molecules27134235
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author Orlandin, Andrea
Guryanov, Ivan
Ferrazzano, Lucia
Biondi, Barbara
Biscaglia, Francesca
Storti, Claudia
Rancan, Marzio
Formaggio, Fernando
Ricci, Antonio
Cabri, Walter
author_facet Orlandin, Andrea
Guryanov, Ivan
Ferrazzano, Lucia
Biondi, Barbara
Biscaglia, Francesca
Storti, Claudia
Rancan, Marzio
Formaggio, Fernando
Ricci, Antonio
Cabri, Walter
author_sort Orlandin, Andrea
collection PubMed
description The suppression of side reactions is one of the most important objectives in peptide synthesis, where highly reactive compounds are involved. Recently, the violuric acid derivative Oxyma-B was introduced into peptide synthesis protocols as a promising additive to efficiently control the optical purity of the amino acids prone to racemization. However, we discovered a side reaction involving the Beckmann rearrangement of Oxyma-B during the coupling reaction, which compromises the yield and purity of the target peptides. Here, we present the investigation of the mechanism of this rearrangement and the optimization of the coupling reaction conditions to control it. These results can be taken into account for the design of novel efficient oxime-based coupling reagents.
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spelling pubmed-92681722022-07-09 Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis Orlandin, Andrea Guryanov, Ivan Ferrazzano, Lucia Biondi, Barbara Biscaglia, Francesca Storti, Claudia Rancan, Marzio Formaggio, Fernando Ricci, Antonio Cabri, Walter Molecules Article The suppression of side reactions is one of the most important objectives in peptide synthesis, where highly reactive compounds are involved. Recently, the violuric acid derivative Oxyma-B was introduced into peptide synthesis protocols as a promising additive to efficiently control the optical purity of the amino acids prone to racemization. However, we discovered a side reaction involving the Beckmann rearrangement of Oxyma-B during the coupling reaction, which compromises the yield and purity of the target peptides. Here, we present the investigation of the mechanism of this rearrangement and the optimization of the coupling reaction conditions to control it. These results can be taken into account for the design of novel efficient oxime-based coupling reagents. MDPI 2022-06-30 /pmc/articles/PMC9268172/ /pubmed/35807480 http://dx.doi.org/10.3390/molecules27134235 Text en © 2022 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Orlandin, Andrea
Guryanov, Ivan
Ferrazzano, Lucia
Biondi, Barbara
Biscaglia, Francesca
Storti, Claudia
Rancan, Marzio
Formaggio, Fernando
Ricci, Antonio
Cabri, Walter
Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis
title Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis
title_full Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis
title_fullStr Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis
title_full_unstemmed Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis
title_short Carbodiimide-Mediated Beckmann Rearrangement of Oxyma-B as a Side Reaction in Peptide Synthesis
title_sort carbodiimide-mediated beckmann rearrangement of oxyma-b as a side reaction in peptide synthesis
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9268172/
https://www.ncbi.nlm.nih.gov/pubmed/35807480
http://dx.doi.org/10.3390/molecules27134235
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