加速硒催化烯丙基和丙炔C-H胺化的机理研究

IF 13.1 1区 化学 Q1 CHEMISTRY, PHYSICAL
Sydney E. Towell, , , Fu-Sheng Wang, , , Daniel R. Godfrey, , and , Aleksandr V. Zhukhovitskiy*, 
{"title":"加速硒催化烯丙基和丙炔C-H胺化的机理研究","authors":"Sydney E. Towell,&nbsp;, ,&nbsp;Fu-Sheng Wang,&nbsp;, ,&nbsp;Daniel R. Godfrey,&nbsp;, and ,&nbsp;Aleksandr V. Zhukhovitskiy*,&nbsp;","doi":"10.1021/acscatal.5c05099","DOIUrl":null,"url":null,"abstract":"<p >Catalytic allylic and propargylic C–H aminations present valuable opportunities for the late-stage modification of pharmacophores in drug discovery. However, modern methodology is limited by reliance on expensive transition metal catalysts or slow reactivity. While selenium-catalyzed methods avoid some of these issues, in their current state, they require high catalyst loadings (15 mol %), superstoichiometric quantities of the amine and oxidant source, and long reaction times. Furthermore, our understanding of the mechanism remains incomplete: e.g., what is the catalytically active species, how is the precatalyst converted to it, and what is the role of the ligand? In this paper, we report an <i>N</i>-heterocyclic carbene selenide (NHC-Se) that allows for substantially reduced loadings of selenium without sacrificing reaction time, improves conversions and yields for challenging substrates, and even exhibits the capacity to catalyze 1,4-allylic diamination of alkenes. To understand the origin of the enhanced activity compared to the state-of-the-art NHC-Se precatalyst, we conducted a mechanistic study that supports ligand-free selenium diimide as the active enophile in these systems, while the NHC-derived byproducts, like the corresponding urea, facilitate turnover. We also isolate and structurally characterize NHC-Se mono- and diimido species and explore their mechanistic role. Thus, this work advances C–H amination methodology, our understanding of its mechanistic underpinnings, and selenium chemistry at large.</p>","PeriodicalId":9,"journal":{"name":"ACS Catalysis ","volume":"15 19","pages":"16908–16916"},"PeriodicalIF":13.1000,"publicationDate":"2025-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Mechanistic Insights toward Accelerated Selenium-Catalyzed Allylic and Propargylic C–H Amination\",\"authors\":\"Sydney E. Towell,&nbsp;, ,&nbsp;Fu-Sheng Wang,&nbsp;, ,&nbsp;Daniel R. Godfrey,&nbsp;, and ,&nbsp;Aleksandr V. Zhukhovitskiy*,&nbsp;\",\"doi\":\"10.1021/acscatal.5c05099\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >Catalytic allylic and propargylic C–H aminations present valuable opportunities for the late-stage modification of pharmacophores in drug discovery. However, modern methodology is limited by reliance on expensive transition metal catalysts or slow reactivity. While selenium-catalyzed methods avoid some of these issues, in their current state, they require high catalyst loadings (15 mol %), superstoichiometric quantities of the amine and oxidant source, and long reaction times. Furthermore, our understanding of the mechanism remains incomplete: e.g., what is the catalytically active species, how is the precatalyst converted to it, and what is the role of the ligand? In this paper, we report an <i>N</i>-heterocyclic carbene selenide (NHC-Se) that allows for substantially reduced loadings of selenium without sacrificing reaction time, improves conversions and yields for challenging substrates, and even exhibits the capacity to catalyze 1,4-allylic diamination of alkenes. To understand the origin of the enhanced activity compared to the state-of-the-art NHC-Se precatalyst, we conducted a mechanistic study that supports ligand-free selenium diimide as the active enophile in these systems, while the NHC-derived byproducts, like the corresponding urea, facilitate turnover. We also isolate and structurally characterize NHC-Se mono- and diimido species and explore their mechanistic role. Thus, this work advances C–H amination methodology, our understanding of its mechanistic underpinnings, and selenium chemistry at large.</p>\",\"PeriodicalId\":9,\"journal\":{\"name\":\"ACS Catalysis \",\"volume\":\"15 19\",\"pages\":\"16908–16916\"},\"PeriodicalIF\":13.1000,\"publicationDate\":\"2025-09-22\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"ACS Catalysis \",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.acs.org/doi/10.1021/acscatal.5c05099\",\"RegionNum\":1,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, PHYSICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"ACS Catalysis ","FirstCategoryId":"92","ListUrlMain":"https://pubs.acs.org/doi/10.1021/acscatal.5c05099","RegionNum":1,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, PHYSICAL","Score":null,"Total":0}
引用次数: 0

摘要

催化烯丙基和丙炔C-H胺化为药物发现中药物载体的后期修饰提供了宝贵的机会。然而,现代方法受到依赖昂贵的过渡金属催化剂或反应性慢的限制。虽然硒催化方法避免了这些问题,但在目前的状态下,它们需要高催化剂负载(15 mol %),超化学计量量的胺和氧化剂源,以及长反应时间。此外,我们对其机制的理解仍然不完整:例如,什么是催化活性物质,预催化剂如何转化为它,配体的作用是什么?在本文中,我们报道了一种n -杂环硒化碳(NHC-Se),它可以在不牺牲反应时间的情况下大幅减少硒的负荷,提高对挑战性底物的转化率和产率,甚至表现出催化1,4-烯丙基烯烃二化的能力。为了了解与最先进的NHC-Se预催化剂相比活性增强的来源,我们进行了一项机制研究,支持在这些体系中无配体的二亚胺硒作为活性亲烯试剂,而nhc衍生的副产物,如相应的尿素,促进了转化。我们还分离和结构表征NHC-Se单和双胺物种,并探讨其机制作用。因此,这项工作推进了C-H胺化方法,我们对其机制基础的理解,以及硒化学的整体发展。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Mechanistic Insights toward Accelerated Selenium-Catalyzed Allylic and Propargylic C–H Amination

Mechanistic Insights toward Accelerated Selenium-Catalyzed Allylic and Propargylic C–H Amination

Mechanistic Insights toward Accelerated Selenium-Catalyzed Allylic and Propargylic C–H Amination

Catalytic allylic and propargylic C–H aminations present valuable opportunities for the late-stage modification of pharmacophores in drug discovery. However, modern methodology is limited by reliance on expensive transition metal catalysts or slow reactivity. While selenium-catalyzed methods avoid some of these issues, in their current state, they require high catalyst loadings (15 mol %), superstoichiometric quantities of the amine and oxidant source, and long reaction times. Furthermore, our understanding of the mechanism remains incomplete: e.g., what is the catalytically active species, how is the precatalyst converted to it, and what is the role of the ligand? In this paper, we report an N-heterocyclic carbene selenide (NHC-Se) that allows for substantially reduced loadings of selenium without sacrificing reaction time, improves conversions and yields for challenging substrates, and even exhibits the capacity to catalyze 1,4-allylic diamination of alkenes. To understand the origin of the enhanced activity compared to the state-of-the-art NHC-Se precatalyst, we conducted a mechanistic study that supports ligand-free selenium diimide as the active enophile in these systems, while the NHC-derived byproducts, like the corresponding urea, facilitate turnover. We also isolate and structurally characterize NHC-Se mono- and diimido species and explore their mechanistic role. Thus, this work advances C–H amination methodology, our understanding of its mechanistic underpinnings, and selenium chemistry at large.

求助全文
通过发布文献求助,成功后即可免费获取论文全文。 去求助
来源期刊
ACS Catalysis
ACS Catalysis CHEMISTRY, PHYSICAL-
CiteScore
20.80
自引率
6.20%
发文量
1253
审稿时长
1.5 months
期刊介绍: ACS Catalysis is an esteemed journal that publishes original research in the fields of heterogeneous catalysis, molecular catalysis, and biocatalysis. It offers broad coverage across diverse areas such as life sciences, organometallics and synthesis, photochemistry and electrochemistry, drug discovery and synthesis, materials science, environmental protection, polymer discovery and synthesis, and energy and fuels. The scope of the journal is to showcase innovative work in various aspects of catalysis. This includes new reactions and novel synthetic approaches utilizing known catalysts, the discovery or modification of new catalysts, elucidation of catalytic mechanisms through cutting-edge investigations, practical enhancements of existing processes, as well as conceptual advances in the field. Contributions to ACS Catalysis can encompass both experimental and theoretical research focused on catalytic molecules, macromolecules, and materials that exhibit catalytic turnover.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:604180095
Book学术官方微信