Electrochemical Driven Decarboxylative Fluorination of α‐Ketoacids

Acyl fluorides are valuable acyl transfer platforms owing to their unique reactivity and stability; however, their preparation often requires specialized fluorinating reagents, metal catalysts, or stoichiometric oxidants. Herein, we report an electrocatalytic decarboxylative fluorination of α‐ketoacids for the synthesis of acyl fluorides using inexpensive triethylamine trihydrofluoride (Et 3 N·3HF) as both the fluoride source and supporting electrolyte. Mechanistic studies support a pathway involving anodically generated acyl radicals that undergo further oxidation to acylium ions before fluoride trapping. This protocol features mild reaction conditions, broad substrate scope, excellent functional‐group tolerance, and gram‐scale applicability, providing a practical, economical, and sustainable approach to acyl fluorides from readily available α‐ketoacids.