Abstract: The first synthesis of acetylenic carboxylates is reported. Reaction of PhI (OCOR')* with lithium acetylides, or anion exchange of alkynylphenyliodonium tosylates, gives alkynylphenyliodonium carboxylates that readily decompose to the desired acetylenic carboxylates and iodobenzene. The new acetylenic carboxylates are characterized by spectral means and show unique IR and C-13 absorptions. The scope and limitations of ...