Maloney T Parker, Dohoda Alexander F, Zhu Alec C, Michael Forrest E
University of Washington, Department of Chemistry Box 351700 Seattle Washington 98195-1700 USA
Chem Sci. 2022 Jan 27;13(7):2121-2127. doi: 10.1039/d1sc07067c. eCollection 2022 Feb 16.
Herein we report an intermolecular propargylic C-H amination of alkynes. This reaction is operationally convenient and requires no transition metal catalysts or additives. Terminal, silyl, and internal alkynes bearing a wide range of functional groups can be aminated in high yields. The regioselectivity of amination for unsymmetrical internal alkynes is strongly influenced by substitution pattern (tertiary > secondary > primary) and by relatively remote heteroatomic substituents. We demonstrate that amination of alkynes bearing α-stereocenters occurs with retention of configuration at the newly-formed C-N bond. Competition experiments between alkynes, kinetic isotope effects, and DFT calculations are performed to confirm the mechanistic hypothesis that initial ene reaction of a selenium bis(imide) species is the rate- and product-determining step. This ene reaction has a transition state that results in substantial partial positive charge development at the carbon atom closer to the amination position. Inductive and/or hyperconjugative stabilization or destabilization of this positive charge explains the observed regioselectivities.
在此,我们报道了一种炔烃的分子间烯丙基C-H胺化反应。该反应操作简便,无需过渡金属催化剂或添加剂。带有各种官能团的末端炔烃、硅基炔烃和内炔烃都能以高产率进行胺化反应。不对称内炔烃胺化反应的区域选择性受取代模式(叔碳>仲碳>伯碳)和相对较远的杂原子取代基的强烈影响。我们证明,带有α-立体中心的炔烃胺化反应在新形成的C-N键处构型保持不变。进行了炔烃之间的竞争实验、动力学同位素效应实验和密度泛函理论计算,以证实机理假设,即硒双(亚胺)物种的初始烯反应是速率和产物决定步骤。该烯反应具有一个过渡态,导致在靠近胺化位置的碳原子上产生大量部分正电荷。这种正电荷的诱导和/或超共轭稳定或去稳定作用解释了观察到的区域选择性。