Air‐Insensitive Sulfonylation Enabled by a MOF‐Supported Nickel Photocatalyst

Photoredox nickel dual catalysis has become a powerful tool in organic synthesis over the past decade, demonstrating versatile reactivity and utilizing earth-abundant metals to form new bonds. However, the requirement for strict inert-gas protection and the existence of intricate metal complex equilibria in homogeneous systems present obstacles to further advancement in practical applications and mechanistic studies. Herein, a heterogeneous strategy is devised by immobilizing nickel complexes within a highly crystalline mesoporous framework, enabling the photoinduced sulfonylation of aryl halides to proceed under ambient air conditions. Notably, pre-treatment with coordinating solvents significantly enhances the activity of the framework-supported nickel catalyst. This research not only broadens the scope of sustainable cross-coupling methodologies but also provides valuable insights into designing robust heterogeneous photocatalytic systems.