Diiodotrifluoromethoxylation of Terminal Alkynes

Given the unique properties of the trifluoromethoxy (OCF₃) group and the broad utility of alkenes, synthesis of trifluoromethoxylated alkenes, particularly those incorporating halogen substituents, is of significant importance. While chloro-/bromo-trifluoromethoxylated alkenes are established, iodo variants remain underdeveloped (single example, 18% yield). We herein present diiodotrifluoromethoxylation of terminal alkynes, delivering 1,1-diiodo-2-(OCF₃)-alkenes in 61-92% yields. This method features a broad substrate scope and scalability and enables late-stage functionalization of bioactive molecules.