Muller Cyprien, Horký Filip, Vayer Marie, Golushko Andrei, Lebœuf David, Moran Joseph
Institut de Science et d'Ingénierie Supramoléculaires (ISIS), CNRS UMR 7006, Université de Strasbourg 8 allée Gaspard Monge 67000 Strasbourg France
Chem Sci. 2023 Feb 15;14(11):2983-2989. doi: 10.1039/d2sc06692k. eCollection 2023 Mar 15.
The oxa-Pictet-Spengler reaction is arguably the most straightforward and modular way to construct the privileged isochroman motif, but its scope is largely limited to benzaldehyde derivatives and to electron-rich β-phenylethanols that lack substitution along the aliphatic chain. Here we describe a variant of this reaction starting from an epoxide, rather than an aldehyde, that greatly expands the scope and rate of the reaction (<1 h, 20 °C). Besides facilitating the initial Meinwald rearrangement, the use of hexafluoroisopropanol (HFIP) as a solvent expands the electrophile scope to include partners equivalent to ketones, aliphatic aldehydes, and phenylacetyl aldehydes, and the nucleophile scope to include modestly electronically deactivated and highly substituted β-phenylethanols. The products could be easily further derivatised in the same pot by subsequent ring-opening, reductions, and intra- and intermolecular Friedel-Crafts reactions, also in HFIP. Finally, owing to the high pharmacological relevance of the isochroman motif, the synthesis of drug analogues was demonstrated.
氧杂-Pictet-Spengler反应可以说是构建具有特权的异色满基序最直接且模块化的方法,但其适用范围在很大程度上仅限于苯甲醛衍生物以及脂肪链上无取代的富电子β-苯乙醇。在此,我们描述了该反应的一种变体,它从环氧化物而非醛开始,极大地扩展了反应的适用范围和速率(20℃下<1小时)。除了促进初始的Meinwald重排外,使用六氟异丙醇(HFIP)作为溶剂将亲电试剂的范围扩展到包括等同于酮、脂肪醛和苯乙酰醛的底物,并且将亲核试剂的范围扩展到包括电子适度钝化和高度取代的β-苯乙醇。产物可以在同一反应釜中通过随后的开环、还原以及分子内和分子间的Friedel-Crafts反应(同样在HFIP中)轻松地进一步衍生化。最后,由于异色满基序具有高度的药理学相关性,因此展示了药物类似物的合成。