Vine Logan E, Reeves Ryan D, Landwehr Eleanor M, Fernández Israel, Schomaker Jennifer M
Department of Chemistry, 1101 University Avenue, Madison, WI 53706.
Departamento de Orgánica I and Centro de Innovación en Química Avanzada (ORFEO-CINQA), Facultad de Ciencias Químicas, Universidad Complutense de Madrid, 28040 Madrid, Spain.
ACS Catal. 2021 Aug 6;11(15):9485-9494. doi: 10.1021/acscatal.1c01847. Epub 2021 Jul 15.
Pd-catalyzed transformations of allenyl malonates provide convenient access to functionalized carbocycles, but the influence of the ligand, solvent, base, and reaction conditions on the mechanism, regioselectivity, and product outcome of the cyclization are not well-understood. Additionally, from the perspective of synthetic utility, access to either fully substituted or enantioenriched cyclopentane building blocks has not yet been achieved. This work describes how targeted changes to the reaction conditions enable predictable control over the mechanism of Pd-catalyzed allene cross-coupling/cyclization and cycloisomerization, irrespective of the allene substitution pattern. Both enantioenriched cyclopropanes and cyclopentenes can be obtained through axis-to-center chirality transfer from the allene precursor at room temperature, which is not possible using reported Pd-catalyzed methods that result in racemization of the allene. Finally, the ability to divert the reactivity of the allenyl malonate from cross-coupling/cyclization to cycloisomerization by a simple switch of the ligand on Pd from a bidentate phosphine to an electron-poor triphenylphosphite is demonstrated.
钯催化的丙二烯基丙二酸酯转化反应为合成官能化碳环提供了便捷途径,但配体、溶剂、碱和反应条件对环化反应的机理、区域选择性和产物结果的影响尚未得到充分理解。此外,从合成实用性的角度来看,尚未实现获得全取代或对映体富集的环戊烷结构单元的目标。本文描述了如何通过有针对性地改变反应条件,实现对钯催化的丙二烯交叉偶联/环化反应和环异构化反应机理的可预测控制,而与丙二烯的取代模式无关。在室温下,通过丙二烯前体的轴到中心的手性转移,可以得到对映体富集的环丙烷和环戊烯,而使用已报道的导致丙二烯外消旋化的钯催化方法则无法实现这一点。最后,证明了通过简单地将钯上的配体从双齿膦切换为贫电子的亚磷酸三苯酯,能够使丙二烯基丙二酸酯的反应活性从交叉偶联/环化反应转向环异构化反应。