Asymmetric radical NHC organocatalysis-enabled highly enantioselective acylation of inert C(sp<sup>2</sup>)─C(sp<sup>3</sup>) bonds.

Li, Qing-Zhu; He, Mei-Hao; Wang, Peng-Tao; Hong, Long-Hai; Qi, Ting; Kou, Xin-Xin; Xiang, Dong-Yang; Liu, Wan-Cong et al. · Sci Adv · 2026

basic_science · Level V

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Abstract

The pursuit of high enantioselectivity remains a central challenge in the burgeoning area of radical <i>N</i>-heterocyclic carbene (NHC) catalysis. Moreover, direct functionalizations of unstrained and unpolarized C─C bonds continue to pose a formidable obstacle in organocatalysis. Herein, we disclose an asymmetric NHC organocatalytic platform that achieves highly enantioselective radical acylation of inert C(sp<sup>2</sup>)─C(sp<sup>3</sup>) bonds. Central to this advance is the development of a previously unknown collection of chiral thiazolium catalysts integrating medium-ring backbones with <i>C</i><sub>2</sub>-symmetric chiral units, which facilitate the stereoselective acylation of C─C bonds through a Smiles-type rearrangement. This organocatalytic protocol affords more than 70 examples with outstanding yields (up to 99%) and excellent regioselectivity (up to 99:1 rr) and enantioselectivity (up to 99.5:0.5 er) under transition metal-free and light-free conditions. The practicality of this strategy is further underscored by stereo-controlled late-stage functionalization of complex bioactive molecules. Mechanistic insights from combined experimental and computational studies support a radical-mediated catalytic cycle and elucidate the origin of enantioselectivity.