Oleksandr S. Liashuk, Oleksandr P. Demchuk, Oleksandr V. Hryshchuk and Oleksandr O. Grygorenko*,
{"title":"2,5-二氢-1H-吡咯-3-基硼烷衍生物:多克合成和偶联反应","authors":"Oleksandr S. Liashuk, Oleksandr P. Demchuk, Oleksandr V. Hryshchuk and Oleksandr O. Grygorenko*, ","doi":"10.1021/acs.oprd.3c00454","DOIUrl":null,"url":null,"abstract":"<p >A protocol for the multigram synthesis of 3-substituted 2,5-dihydro-1<i>H</i>-pyrrole boronic derivatives is reported. The method relied on the triflation of <i>N</i>-Boc-3-oxopyrrolidine and subsequent palladium-catalyzed borylation. Optimization studies demonstrated the high efficiency of <i>t</i>-BuOK as a base for the triflation step and good performance of the one-pot protocol as compared with the conventional step-by-step synthesis. The method allowed the production of up to 60 g of the target compound (as pure trifluoroborate or technical-grade boropinacolate) in one run using commercially available reagents and common laboratory equipment. Application of the obtained building block for the preparation of compounds relevant to medicinal chemistry through C–C coupling reactions is also illustrated. It is suggested that the boropinacolate form of the title building block is advantageous when immediate synthesis of the coupling products is envisaged, whereas trifluoroborate is more convenient for storage and commercialization.</p>","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":"28 4","pages":"1061–1069"},"PeriodicalIF":3.5000,"publicationDate":"2024-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"2,5-Dihydro-1H-pyrrol-3-yl Boronic Derivatives: Multigram Synthesis and Coupling Reactions\",\"authors\":\"Oleksandr S. Liashuk, Oleksandr P. Demchuk, Oleksandr V. Hryshchuk and Oleksandr O. Grygorenko*, \",\"doi\":\"10.1021/acs.oprd.3c00454\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >A protocol for the multigram synthesis of 3-substituted 2,5-dihydro-1<i>H</i>-pyrrole boronic derivatives is reported. The method relied on the triflation of <i>N</i>-Boc-3-oxopyrrolidine and subsequent palladium-catalyzed borylation. Optimization studies demonstrated the high efficiency of <i>t</i>-BuOK as a base for the triflation step and good performance of the one-pot protocol as compared with the conventional step-by-step synthesis. The method allowed the production of up to 60 g of the target compound (as pure trifluoroborate or technical-grade boropinacolate) in one run using commercially available reagents and common laboratory equipment. Application of the obtained building block for the preparation of compounds relevant to medicinal chemistry through C–C coupling reactions is also illustrated. It is suggested that the boropinacolate form of the title building block is advantageous when immediate synthesis of the coupling products is envisaged, whereas trifluoroborate is more convenient for storage and commercialization.</p>\",\"PeriodicalId\":55,\"journal\":{\"name\":\"Organic Process Research & Development\",\"volume\":\"28 4\",\"pages\":\"1061–1069\"},\"PeriodicalIF\":3.5000,\"publicationDate\":\"2024-03-13\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Organic Process Research & Development\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.acs.org/doi/10.1021/acs.oprd.3c00454\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, APPLIED\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Organic Process Research & Development","FirstCategoryId":"92","ListUrlMain":"https://pubs.acs.org/doi/10.1021/acs.oprd.3c00454","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, APPLIED","Score":null,"Total":0}
2,5-Dihydro-1H-pyrrol-3-yl Boronic Derivatives: Multigram Synthesis and Coupling Reactions
A protocol for the multigram synthesis of 3-substituted 2,5-dihydro-1H-pyrrole boronic derivatives is reported. The method relied on the triflation of N-Boc-3-oxopyrrolidine and subsequent palladium-catalyzed borylation. Optimization studies demonstrated the high efficiency of t-BuOK as a base for the triflation step and good performance of the one-pot protocol as compared with the conventional step-by-step synthesis. The method allowed the production of up to 60 g of the target compound (as pure trifluoroborate or technical-grade boropinacolate) in one run using commercially available reagents and common laboratory equipment. Application of the obtained building block for the preparation of compounds relevant to medicinal chemistry through C–C coupling reactions is also illustrated. It is suggested that the boropinacolate form of the title building block is advantageous when immediate synthesis of the coupling products is envisaged, whereas trifluoroborate is more convenient for storage and commercialization.
期刊介绍:
The journal Organic Process Research & Development serves as a communication tool between industrial chemists and chemists working in universities and research institutes. As such, it reports original work from the broad field of industrial process chemistry but also presents academic results that are relevant, or potentially relevant, to industrial applications. Process chemistry is the science that enables the safe, environmentally benign and ultimately economical manufacturing of organic compounds that are required in larger amounts to help address the needs of society. Consequently, the Journal encompasses every aspect of organic chemistry, including all aspects of catalysis, synthetic methodology development and synthetic strategy exploration, but also includes aspects from analytical and solid-state chemistry and chemical engineering, such as work-up tools,process safety, or flow-chemistry. The goal of development and optimization of chemical reactions and processes is their transfer to a larger scale; original work describing such studies and the actual implementation on scale is highly relevant to the journal. However, studies on new developments from either industry, research institutes or academia that have not yet been demonstrated on scale, but where an industrial utility can be expected and where the study has addressed important prerequisites for a scale-up and has given confidence into the reliability and practicality of the chemistry, also serve the mission of OPR&D as a communication tool between the different contributors to the field.