Institut für Organische Chemie, Eberhard Karls Universität Tübingen, Auf der Morgenstelle 18, 72076, Tübingen, Germany.
ChemistryOpen. 2022 Oct;11(10):e202200015. doi: 10.1002/open.202200015. Epub 2022 Feb 26.
The generation of the quaternary stereocenter at the C9 position of salvinorin A precursors by the Claisen rearrangement was investigated. The required allyl alcohol was prepared from a Wieland-Miescher ketone using a known γ-hydroxylation, reduction of the enone double bond, cyanohydrin formation, and elimination, yielding an unsaturated nitrile. A two-step reduction led to the required allyl alcohol. The subsequent Johnson-Claisen rearrangement provided a mixture of two diastereomeric 1,4-unsaturated esters in a ratio of around 2.6 : 1. The major isomer could be converted to a key intermediate of the Hagiwara synthesis of salvinorin A.
我们研究了通过克莱森重排在 Salvinorin A 前体的 C9 位生成季立体中心。所需的烯丙醇是由 Wieland-Miescher 酮使用已知的γ-羟化、烯酮双键还原、氰醇形成和消除反应制备的,得到不饱和腈。两步还原得到所需的烯丙醇。随后的约翰逊-克莱森重排提供了两种非对映异构体的 1,4-不饱和酯的混合物,比例约为 2.6∶1。主要异构体可以转化为 Hagiwara 合成 Salvinorin A 的关键中间体。