Department of Chemistry, Massachusetts Institute of Technology, 77 Massachusetts Ave., Cambridge, Massachusetts 02139, United States.
Acc Chem Res. 2020 Jun 16;53(6):1229-1243. doi: 10.1021/acs.accounts.0c00164. Epub 2020 May 13.
In organic synthesis, ligand-modified copper(I) hydride (CuH) complexes have become well-known reagents and catalysts for selective reduction, particularly toward Michael acceptors and carbonyl compounds. Recently, our group and others have found that these hydride complexes undergo migratory insertion (hydrocupration) with relatively unactivated and electronically unpolarized olefins, producing alkylcopper intermediates that can be leveraged to forge a variety of useful bonds. The resulting formal hydrofunctionalization reactions have formed the basis for a resurgence of research in CuH catalysis. This Account chronicles the development of this concept in our research group, highlighting its origin in the context of asymmetric hydroamination, evolution to more general C-X bond-forming reactions, and applications in the addition of olefin-derived nucleophiles to carbonyl derivatives.Hydroamination, the formal insertion of an olefin into the N-H bond of an amine, is a process of significant academic and industrial interest, due to its potential to transform widely available alkenes and alkynes into valuable complex amines. We developed a polarity-reversed strategy for catalytic enantioselective hydroamination relying on the reaction of olefins with CuH to generate chiral organocopper intermediates, which are intercepted by electrophilic amine reagents. By engineering the auxiliary ligand, amine electrophile, and reaction conditions, the scope of this method has since been extended to include many types of olefins, including challenging internal olefins. Further, the scope of amine reagents has been expanded to enable the synthesis of primary, secondary, and tertiary amines as well as amides, N-alkylated heterocycles, and anilines. All of these reactions exhibit high regio- and stereoselectivity and, due to the mild conditions required, excellent tolerance for heterocycles and polar functional groups.Though the generation of alkylcopper species from olefins was originally devised as a means to solve the hydroamination problem, we soon found that these intermediates could react efficiently with an unexpectedly broad range of electrophiles, including alkyl halides, silicon reagents, arylpalladium species, heterocycles, and carbonyl derivatives. The general ability of olefins to function as precursors for nucleophilic intermediates has proved particularly advantageous in carbonyl addition reactions because it overcomes many of the disadvantages associated with traditional organometallic reagents. By removing the need for pregeneration of the nucleophile in a separate operation, CuH-catalyzed addition reactions of olefin-derived nucleophiles feature improved step economy, enhanced functional group tolerance, and the potential for catalyst control over regio- and stereoselectivity. Following this paradigm, feedstock olefins such as allene, butadiene, and styrene have been employed as reagents for asymmetric alkylation of ketones, imines, and aldehydes.
在有机合成中,配体修饰的铜(I)氢化物(CuH)配合物已成为用于选择性还原的知名试剂和催化剂,特别是对于迈克尔受体和羰基化合物。最近,我们小组和其他小组发现,这些氢化物配合物与相对非活化和电子非极化的烯烃进行迁移插入(氢铜化),生成可以利用的烷基铜中间体,从而可以形成各种有用的键。由此产生的形式氢官能化反应为 CuH 催化的研究复兴奠定了基础。本说明记录了我们小组在这一概念上的发展,重点介绍了它在不对称氢氨化背景下的起源、向更通用的 C-X 键形成反应的演变以及在烯烃衍生亲核试剂与羰基衍生物加成中的应用。氢氨化,即烯烃正式插入胺的 N-H 键中,是一个具有重要学术和工业意义的过程,因为它有可能将广泛存在的烯烃和炔烃转化为有价值的复杂胺。我们开发了一种基于 CuH 与烯烃反应生成手性有机铜中间体,然后被亲电胺试剂捕获的极性反转策略,用于催化对映选择性氢氨化。通过设计辅助配体、胺亲电试剂和反应条件,该方法的范围已经扩展到包括许多类型的烯烃,包括具有挑战性的内烯烃。此外,胺试剂的范围已经扩大,能够合成伯、仲和叔胺以及酰胺、N-烷基化杂环和苯胺。所有这些反应都表现出高区域和立体选择性,并且由于所需的温和条件,对杂环和极性官能团具有极好的耐受性。虽然从烯烃生成烷基铜物种最初被设计为解决氢氨化问题的一种手段,但我们很快发现这些中间体可以与广泛的亲电试剂有效地反应,包括烷基卤化物、硅试剂、芳基钯物种、杂环和羰基衍生物。烯烃作为亲核中间体前体的一般能力在羰基加成反应中特别有利,因为它克服了与传统有机金属试剂相关的许多缺点。通过消除在单独操作中预先生成亲核试剂的需要,CuH 催化的烯烃衍生亲核试剂的加成反应具有提高的步骤经济性、增强的官能团耐受性以及催化剂对区域和立体选择性的控制潜力。遵循这一范例,丙烯、丁二烯和苯乙烯等原料烯烃已被用作酮、亚胺和醛的不对称烷基化试剂。