Tandem Photooxidation/Acetalization of Alcohols to Acetals/Ketals with Sulfur‐doped Carbon Nitride

Abstract Selective chemical synthesis using visible light is challenging. Herein we present photooxidation and subsequent acetalization of alcohols in tandem with high selectivity employing sulfur‐doped polymeric carbon nitride (CNS) under mild conditions. Distinctive electronic structure of CNS allows it to efficiently catalyze the oxidation of alcohols and subsequent acetalization of the obtained products with primary alcohols introduced at the outset. The process is green, utilizes visible light and air, and has a broad substrate scope with good activity and selectivity. Catalytic system works without any significant loss in activity after multiple reaction cycles, offers a sustainable way to produce a variety of acetals/ketals for green synthesis applications.