Visible‐Light‐Mediated Regioselective Trichloromethyl Hydroxylation of Alkenes: A Metal‐Free Strategy for β‐Trichloromethyl Alcohols

Abstract A visible light‐driven, metal‐free strategy for the regioselective synthesis of β‐trichloromethyl alcohols has been developed through a three‐component reaction of alkenes with CCl 4 and TBHP under mild blue LED irradiation. This method achieves vicinal trichloromethyl hydroxylation with broad substrate scope and good functional group tolerance. Mechanistic studies revealed a radical pathway in which TBHP acts as the hydroxyl donor. The protocol operates under ambient conditions without transition metals, offering a sustainable and scalable platform for synthesizing polyhalogenated building blocks with potential applications in medicinal chemistry and synthetic transformations.