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Photoredox/Nickel Dual Catalysis for C(sp<sup>2</sup>)–C(sp<sup>3</sup>) Cross-Electrophile Coupling Reaction of Mesylates of Phenols and Primary Alcohols

Sayan K. Jana, R. N. Bhattacharya, Purusattam Dey, Sunit Chakraborty, Biplab Maji

2024ACS Catalysis16 citationsDOI

Abstract

Introducing alkyl groups, particularly through innovative C(sp 2 )–C(sp 3 ) bond-forming methods utilizing abundant feedstocks, holds promise for expanding chemical space, especially in drug discovery programs. Herein, we employed biomass-derived abundant phenols and unactivated aliphatic alcohols as the coupling partners for C(sp 2 )–C(sp 3 ) cross-electrophile coupling reactions. Our innovation involved activating both the coupling partner via the same activator and designing a catalytic system that activates stronger bonds while ensuring cross-selectivity. The visible-light photoredox/nickel dual catalytic systems accommodate a large substrate scope tolerating diverse functional groups. Besides, both the activation and cross-coupling reactions could be performed in one pot, and the reaction could be scaled up. The method was also executed for iterative cross-coupling and applied for the late-stage functionalization of drug molecules, highlighting their synthetic applicability. Preliminary mechanistic studies involving luminescence quenching, cyclic voltammetry, radical quenching, and radical clock studies elucidated the proposed reaction mechanism.

Topics & Concepts

CatalysisNickelElectrophileChemistryPrimary (astronomy)PhenolsCoupling (piping)Coupling reactionMedicinal chemistryPhotochemistryOrganic chemistryMaterials sciencePhysicsMetallurgyAstronomyRadical Photochemical ReactionsSulfur-Based Synthesis TechniquesCatalytic Cross-Coupling Reactions