Organophotoredox‐Catalyzed Oxyalkylation–Peroxidation of Alkenes With Ethers and <i>Tert</i> ‐Butyl Hydroperoxide

We report a visible‐light‐induced three‐component peroxidation of alkenes with ethers and tert ‐butyl hydroperoxide (TBHP) using Rhodamine B as an organophotoredox catalyst. This environmentally friendly protocol provides efficient access to a variety of multisubstituted tert ‐butyl peroxides. The resulting tert ‐butylperoxy group can be selectively converted into carbonyl or hydroxyl groups under mild conditions, highlighting the synthetic utility of this peroxidation strategy.