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Iodine-Catalyzed Radical C–H Amination of Nonaromatic Imidazole Oxides: Access to Cyclic α-Aminonitrones

Alexey A. Akulov, Михаил В. Вараксин, Anna A. Nelyubina, Anton N. Tsmokaluk, Dmitrii G. Mazhukin, А. Ya. Tikhonov, Valery N. Charushin, Олег Н. Чупахин

2023The Journal of Organic Chemistry13 citationsDOI

Abstract

A straightforward cross-dehydrogenative coupling approach to incorporate alicyclic amino residues into the structure of model cyclic aldonitrones, 2 H -imidazole oxides, is reported. The elaborated C(sp 2 )–H functionalization is achieved by employing cyclic amines in the presence of the I 2 – tert -butyl hydroperoxide (TBHP) reagent system. As a result, a series of 19 novel heterocyclic derivatives were obtained in yields of up to 97%. A mechanistic study involving electron paramagnetic resonance spectroscopic experiments allowed the radical nature of the reaction to be confirmed. In particular, the envisioned mechanistic rationale comprises N-iodination of a cyclic amine, followed by N–I bond homolysis of the resulting intermediate and subsequent amination of the nitrone moiety via the newly generated nitrogen-centered radical.

Topics & Concepts

ChemistryAminationHomolysisImidazoleCyclic aminesAmine gas treatingElectron paramagnetic resonanceMoietyReagentCatalysisAlicyclic compoundNitroneMedicinal chemistryOrganic chemistryPhotochemistryRadicalCycloadditionPhysicsNuclear magnetic resonanceCatalytic C–H Functionalization MethodsOxidative Organic Chemistry ReactionsRadical Photochemical Reactions
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