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C(<i>sp</i><sup>3</sup>)−C(<i>sp</i><sup>3</sup>) Bond Formation <i>via</i> Electrochemical Alkoxylation and Subsequent Lewis Acid Promoted Reactions

Enol López, Carlo van Melis, Raúl Martín, Alessia Petti, Antonio de la Hoz, Ángel Díaz‐Ortiz, Adrian P. Dobbs, Kevin Lam, Jesús Alcázar

2021Advanced Synthesis & Catalysis13 citationsDOI

Abstract

Abstract A two‐step transition metal‐free methodology for the C( sp 3 )−C( sp 3 ) functionalisation of saturated N ‐heterocyclic systems is disclosed. First, aminal derivatives are generated through the anodic oxidation of readily accessible carboxylic acids. Then, in the presence of BF 3 ⋅ OEt 2 , iminium ions are unmasked and rapidly alkylated by organozinc reagents under flow conditions. Secondary, tertiary and quaternary carbon centers have been successfully assembled using this methodology. Such an approach is especially relevant to drug discovery since it increases C( sp 3 )‐functionalities rapidly within a molecular framework. As proof of concept, our methodology was applied to derivatization of peptides and an API. magnified image

Topics & Concepts

ChemistryIminiumReagentDerivatizationAminalElectrochemistryTransition metalLewis acids and basesLithium (medication)Combinatorial chemistryAlkylationMedicinal chemistryOrganic chemistryIonHigh-performance liquid chromatographyCatalysisElectrodeEndocrinologyPhysical chemistryMedicineRadical Photochemical ReactionsCatalytic C–H Functionalization MethodsChemical Synthesis and Analysis