Enamine Ltd, 78 Chervonotkatska str., Kyiv 02094, Ukraine.
Taras Shevchenko National University of Kyiv, 60 Volodymyrska str., Kyiv 01033, Ukraine.
J Org Chem. 2021 Jun 4;86(11):7333-7346. doi: 10.1021/acs.joc.1c00148. Epub 2021 May 27.
The convenient and scalable preparative approach for the two-step α-methylation of ketones is described. The optimized protocols for regioselective preparation of enaminones with further diastereoselective and functional groups tolerant hydrogenation to α-methylketones are developed. The scope and limitations of the proposed methodology are discussed. The advantages compared to known procedures are demonstrated. The unexpected role of acetone in the hydrogenation is suggested. The evaluation of the method for both early building block synthesis and late-stage CH-functionalization is shown. The elaborate procedures' preparability and scalability are demonstrated by the synthesis of several α-methyl ketones up to 100 g amount.
描述了酮的两步α-甲基化的便捷和可扩展的制备方法。开发了用于区域选择性制备烯胺酮的优化方案,进一步具有对非对映选择性和官能团容忍的加氢以得到α-甲基酮。讨论了所提出方法的范围和限制。与已知程序相比,证明了其优势。提出了在加氢中丙酮的意外作用。显示了该方法在早期构建块合成和后期 CH 官能化中的评估。通过合成几种α-甲基酮至 100 g 量,证明了详细程序的可制备性和可扩展性。