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A one‐pot protocol was developed for the synthesis of unsymmetrical 1,3‐butadiynes. The procedure is based on two sequential reactions: deprotection of R–C≡C–C≡C–C(Me)2OH derivatives in a retro‐Favorskii reaction to furnish a terminal 1,3‐butadiyne compound, which reacted with aryl iodides in a Sonogashira‐type cross‐coupling reaction catalyzed by Pd(PPh3)4 and CuI, using TBAOH as activator and toluene...