Obregón Erlaitz B, Rost Louise G, Kocemba Ida R, Kristensen Anne, McLeod David A, Jørgensen Karl Anker
Department of Chemistry, Aarhus University, 8000, Aarhus C, Denmark.
Angew Chem Int Ed Engl. 2024 Oct 14;63(42):e202410524. doi: 10.1002/anie.202410524. Epub 2024 Sep 5.
The substituted tetrahydrofuran core is a structural motif in many biologically active and natural compounds. However, the scarcity of enantioselective methods developed towards its synthesis makes this field challenging and attractive to explore. Herein, the first Brønsted-base catalyzed enantioselective (3+2) annulation of donor-acceptor cyclopropanes with aldehydes and ketones affording enantioenriched 2,3,5-substituted tetrahydrofurans is reported. The reaction concept is based on activation of racemic β-cyclopropyl ketones by a chiral bifunctional Brønsted base which catalyzes the (3+2) annulation for a range of aldehydes and ketones. For aldehydes, the annulation furnished tetrahydrofurans in excellent yield, good diastereoselectivity and with excellent enantioselectivity up to >99 % ee. Surprisingly, aromatic aldehydes afforded the cis-2,5-substituted tetrahydrofurans as the major diastereoisomer, while for aliphatic aldehydes the trans-cycloadduct was favored. The reaction also proceeds well for ketones affording spiro tetrahydrofurans in excellent yields and enantioselectivities (up to 99 % ee). Hammett studies have been conducted to elucidate the influence of the electronic nature of benzaldehydes on the stereoselectivity. Based on the diastereochemical outcome for the aldehydes, two reaction paths for aromatic and aliphatic aldehydes are proposed. Finally, two diastereoselective synthetic transformations have been conducted to demonstrate the synthetic potential of the obtained products.
取代四氢呋喃核心结构是许多生物活性化合物和天然化合物中的一种结构基序。然而,针对其合成所开发的对映选择性方法稀缺,使得该领域具有挑战性但又极具探索吸引力。本文报道了首例布朗斯特碱催化供体-受体环丙烷与醛和酮的对映选择性(3+2)环化反应,生成对映体富集的2,3,5-取代四氢呋喃。该反应概念基于手性双功能布朗斯特碱对消旋β-环丙基酮的活化,该碱催化一系列醛和酮的(3+2)环化反应。对于醛,环化反应以优异的产率、良好的非对映选择性和高达>99% ee的优异对映选择性生成四氢呋喃。令人惊讶的是,芳香醛以顺式-2,5-取代四氢呋喃作为主要非对映异构体,而对于脂肪醛,反式环加成产物更受青睐。该反应对于酮也能顺利进行,以优异的产率和对映选择性(高达99% ee)生成螺四氢呋喃。已进行哈米特研究以阐明苯甲醛电子性质对立体选择性的影响。基于醛的非对映化学结果,提出了芳香醛和脂肪醛的两条反应路径。最后,进行了两个非对映选择性合成转化,以证明所得产物的合成潜力。