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The deprotection of a dithioacetal (ProtPE) via visible light photocatalysis (PC) yields the o‐methylbenzaldehyde (o‐MBA). The o‐MBA rearranges to a photoenol (PE) upon UV‐light irradiation, enabling a simultaneous Diels–Alder reaction with N‐ethylmaleimide (NEM). This one‐pot reaction is dual color gated as the deprotection does not occur under UV irradiation and the Diels–Alder reaction does not occur under visible light irradiation.
