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Stannylation of calcium carbide followed by Sn–hypervalent iodine(III) exchange reaction cleanly afforded the electrophilic ethynylating agent ethynyl(phenyl)-λ 3 -iodane in high yield. This two-step method uses very inexpensive materials and is readily operable without any special precautions.

Practical Synthesis of Ethynyl(phenyl)-λ3-Iodane Using Calcium Carbide as an Ethynyl Group Source