Ghasemloo Omid, Hasselbrink Carson L, Cardona Douglas D, DeBoef Brenton, Hayes Dugan
Department of Chemistry, University of Rhode Island, 45 Upper College Rd, Kingston, RI, 02881, USA.
Chemistry. 2025 Jul 11;31(39):e202501531. doi: 10.1002/chem.202501531. Epub 2025 Jun 4.
The oxidation of alcohols, amines, and halides is a fundamental transformation in organic chemistry with significant applications in the synthesis of fine chemicals, pharmaceuticals, and natural products. Here we show that a broad variety of N-heteroarenes bearing hydroxymethyl, aminomethyl, or halomethyl groups are oxidatively dehydrogenated to their respective aldehydes by simply heating them in acidic or basic aqueous solution under ambient atmosphere. The quantitative oxidation of 9-acridinemethanol to 9-acridinecarboxaldehyde serves as an illustrative example, proceeding to completion within 3 hours in refluxing 5% aqueous acetic acid or even household vinegar. Quinoline derivatives may be similarly oxidized but require higher temperatures and longer reaction times, while indole derivatives are oxidized under basic conditions. Based on comprehensive regioselectivity screens, internal kinetic isotope competition, and density functional theory (DFT) calculations, we propose a mechanism in which migration of a methylene hydrogen to the pyridinic nitrogen by acid-catalyzed dearomative tautomerization yields an unstable enol or enamine intermediate that then irreversibly loses two hydrogen atoms to atmospheric oxygen. In addition to the simplicity and environmentally benign nature of our method, we observe no indication of any over-oxidation to carboxylic acids. Finally, we demonstrate the synthetic utility of this reaction through two different one-pot formylations of acridine.
醇、胺和卤化物的氧化是有机化学中的一种基本转化反应,在精细化学品、药物和天然产物的合成中具有重要应用。在此我们表明,通过在环境气氛下于酸性或碱性水溶液中简单加热,多种带有羟甲基、氨基甲基或卤甲基的氮杂芳烃可被氧化脱氢生成各自的醛。9-吖啶甲醇定量氧化为9-吖啶甲醛就是一个典型例子,在5%的醋酸水溶液甚至家用醋中回流3小时即可完成反应。喹啉衍生物也可类似地被氧化,但需要更高的温度和更长的反应时间,而吲哚衍生物则在碱性条件下被氧化。基于全面的区域选择性筛选、内部分子动力学同位素竞争以及密度泛函理论(DFT)计算,我们提出了一种机制,即通过酸催化的去芳香化互变异构,亚甲基氢迁移至吡啶氮原子上,生成一种不稳定的烯醇或烯胺中间体,然后该中间体不可逆地向大气中的氧气失去两个氢原子。除了我们方法的简单性和环境友好性外,我们未观察到任何过度氧化为羧酸的迹象。最后,我们通过吖啶的两种不同的一锅法甲酰化反应展示了该反应的合成实用性。