Department of Chemistry, Merkert Chemistry Center, Boston College, Chestnut Hill, Massachusetts 02467, United States.
Supramolecular Science and Engineering Institute, University of Strasbourg, CNRS, 67000 Strasbourg, France.
J Am Chem Soc. 2020 Oct 21;142(42):18200-18212. doi: 10.1021/jacs.0c08732. Epub 2020 Oct 5.
A widely applicable, practical, and scalable strategy for efficient and enantioselective synthesis of β,γ-unsaturated ketones that contain an α-stereogenic center is disclosed. Accordingly, aryl, heteroaryl, alkynyl, alkenyl, allyl, or alkyl ketones that contain an α-stereogenic carbon with an alkyl, an aryl, a benzyloxy, or a siloxy moiety can be generated from readily available starting materials and by the use of commercially available chiral ligands in 52-96% yield and 93:7 to >99:1 enantiomeric ratio. To develop the new method, conditions were identified so that high enantioselectivity would be attained and the resulting α-substituted NH-ketimines, wherein there is strong C═N → B(pin) coordination, would not epimerize before conversion to the derived ketone by hydrolysis. It is demonstrated that the ketone products can be converted to an assortment of homoallylic tertiary alcohols in 70-96% yield and 92:8 to >98:2 dr-in either diastereomeric form-by reactions with alkyl-, aryl-, heteroaryl-, allyl-, vinyl-, alkynyl-, or propargyl-metal reagents. The utility of the approach is highlighted through transformations that furnish other desirable derivatives and a concise synthesis route affording more than a gram of a major fragment of anti-HIV agents rubriflordilactones A and B and a specific stereoisomeric analogue.
本文公开了一种广泛适用、实用且可扩展的策略,用于高效和对映选择性合成含有α-手性中心的β,γ-不饱和酮。因此,含有α-手性碳原子的芳基、杂芳基、炔基、烯基、烯丙基或烷基酮,可以从易得的起始原料出发,使用商业可得的手性配体,以 52-96%的产率和 93:7 至>99:1 的对映体比率得到。为了开发新方法,确定了条件,以使获得高对映选择性,并且所得的α取代的 NH-亚胺,其中存在强 C═N → B(pin) 配位,在通过水解转化为衍生的酮之前不会外消旋。结果表明,酮产物可以在 70-96%的产率和 92:8 至>98:2 dr 中,以两种非对映异构体的形式,通过与烷基、芳基、杂芳基、烯丙基、乙烯基、炔基或丙炔基金属试剂反应,转化为各种同烯丙基叔醇。该方法的实用性通过转化为其他所需的衍生物和一种简洁的合成路线得到了突出体现,该路线提供了超过一克抗 HIV 药物rubriflordilactones A 和 B 的主要片段和一种特定的立体异构体类似物。