Palladium/Copper Dual Catalysis in the Cross‐Coupling of Stable Diphosphine Disulfides and Terminal Alkynes in the Presence of Molecular Iodine

ABSTRACT A rapid, convenient, one‐pot strategy for the synthesis of 1‐alkynylphosphine sulfides has been developed via Pd/Cu‐catalyzed cross‐coupling between terminal alkynes and P V –I interelement compound generated from the reaction with air‐ and moisture‐stable tetraphenyldiphosphine disulfides and molecular iodine. The transformation proceeds smoothly under mild conditions, completing within 1 h and affording high conversions to the corresponding 1‐alkynylphosphine sulfides in up to 90% yields. This method provides a practical, efficient route to 1‐alkynylphosphine derivatives using air‐ and moisture‐stable reagents, overcoming the limitations of previous strategies.