2,5-二氢-1H-吡咯-3-基硼烷衍生物:多克合成和偶联反应

IF 3.5 3区 化学 Q2 CHEMISTRY, APPLIED
Oleksandr S. Liashuk, Oleksandr P. Demchuk, Oleksandr V. Hryshchuk and Oleksandr O. Grygorenko*, 
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引用次数: 0

摘要

报告了一种多克合成 3-取代的 2,5-二氢-1H-吡咯硼酸衍生物的方法。该方法依赖于 N-Boc-3-oxopyrrolidine 的三氟化反应和随后的钯催化硼酸化反应。优化研究表明,与传统的分步合成法相比,t-BuOK 作为三氟化反应步骤的碱具有很高的效率,而且一锅法的性能良好。该方法使用市售试剂和普通实验室设备,可一次生产多达 60 克的目标化合物(纯三氟硼酸盐或工业级硼频哪醇)。此外,还说明了通过 C-C 偶联反应制备药物化学相关化合物的应用情况。研究表明,当需要立即合成偶联产物时,标题结构单元的硼频哪醇酯形式具有优势,而三氟硼酸盐则更便于储存和商业化。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

2,5-Dihydro-1H-pyrrol-3-yl Boronic Derivatives: Multigram Synthesis and Coupling Reactions

2,5-Dihydro-1H-pyrrol-3-yl Boronic Derivatives: Multigram Synthesis and Coupling Reactions

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.

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来源期刊
CiteScore
6.90
自引率
14.70%
发文量
251
审稿时长
2 months
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.
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