Department of Applied Chemistry, Graduate School of Engineering, Osaka University, Yamadaoka 2-1, Suita, Osaka, 565-0871, Japan.
Chemistry. 2023 Feb 16;29(10):e202203722. doi: 10.1002/chem.202203722. Epub 2023 Jan 26.
Hypervalent iodine-based aminating reagents containing a transferable (diarylmethylene)amino group can be used for the α-amination of simple carbonyl compounds such as esters, amides, and ketones in the presence of a lithium base. The (diarylmethylene)amino groups of the products can be readily modified, thus providing access to primary amines and diarylmethylamines. The developed method features transition-metal-free conditions and a simple one-pot procedure without the need to prepare enolate equivalents separately, thus offering a general and practical approach to the synthesis of a wide variety of α-amino carbonyl compounds. Experimental mechanistic investigations indicate that this amination proceeds through a unique radical coupling of an α-carbonyl radical with an iminyl radical; they are generated through a single-electron transfer between a lithium enolate and the hypervalent iodine reagent.
含有可转移(二芳基亚甲基)氨基的高价碘基氨化试剂可在碱金属锂的存在下用于简单羰基化合物(如酯、酰胺和酮)的α-胺化。产物的(二芳基亚甲基)氨基可以很容易地进行修饰,从而提供仲胺和二芳基甲胺。所开发的方法具有无过渡金属的条件和简单的一锅法程序,无需单独制备烯醇化物等价物,因此为合成各种α-氨基羰基化合物提供了一种通用且实用的方法。实验性的机理研究表明,这种胺化是通过α-羰基自由基与亚胺基自由基的独特自由基偶联进行的;它们是通过锂烯醇化物和高价碘试剂之间的单电子转移生成的。