Chen Weihao, Chen Yang, Gu Xiao, Chen Zaizhu, Ho Chun-Yu
Guangdong Provincial Key Laboratory of Catalysis, Southern University of Science and Technology (SUSTech), Shenzhen, China.
Shenzhen Grubbs Institute, Department of Chemistry, Southern University of Science and Technology (SUSTech), Shenzhen, China.
Nat Commun. 2022 Sep 20;13(1):5507. doi: 10.1038/s41467-022-33163-6.
Transition-metal-catalyzed homogeneous dehydrogenation and isomerization are common organic molecular activation reactions. Palladium hydrides are good olefin isomerization catalysts but are usually short-lived species under redox-active dehydrogenation conditions. Here, we show that Pd-H in the presence of an N-heterocyclic carbene ligand and an alkene regulator enables transfer-dehydroaromatization, avoiding the homo-disproportionation pathway. The desired product is obtained with up to 99:1 selectivity, and the exo-to-endo olefin isomerization can be carried out in one pot. In contrast to previously reported methods that rely on the efficient removal of Pd-H, the approach reported herein benefits from the steric effects of the N-heterocyclic carbene and the choice of alkene to regulate the competing reactivity of allylic C‒H activation and hydropalladation. This method circumvents the challenges associated with tedious olefin separation and a low exo-to-endo olefin isomerization ratio and expands the scope to include challenging endo- and exo-cyclic olefins under mild, neutral, and oxidant-free conditions. Overall, herein, we provide a strategy to synthesize (hetero)aromatic compounds via chemoselective dehydrogenation of cyclic alkenes over ketones and the dehydrogenative Diels-Alder reaction of a cyclic enamine.
过渡金属催化的均相脱氢和异构化是常见的有机分子活化反应。氢化钯是良好的烯烃异构化催化剂,但在氧化还原活性脱氢条件下通常是寿命较短的物种。在此,我们表明,在氮杂环卡宾配体和烯烃调节剂存在下的钯氢能够实现转移脱氢芳构化,避免均歧化途径。以高达99:1的选择性获得所需产物,并且外消旋到内消旋烯烃异构化可以一锅法进行。与先前报道的依赖于有效去除钯氢的方法不同,本文报道的方法受益于氮杂环卡宾的空间效应和烯烃的选择,以调节烯丙基C-H活化和氢化钯化的竞争反应性。该方法规避了与繁琐的烯烃分离和低外消旋到内消旋烯烃异构化比率相关的挑战,并将范围扩展到包括在温和、中性和无氧化剂条件下具有挑战性的内环和外环烯烃。总体而言,本文我们提供了一种通过环状烯烃在酮上的化学选择性脱氢以及环状烯胺的脱氢狄尔斯-阿尔德反应来合成(杂)芳族化合物的策略。