Copper‐Catalyzed Synthesis of Thiosulfonates Using Thiols and Water Through a Radical Process in Air

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Copper‐catalyzed oxidation of thiols under air atmosphere could prepare efficiently the corresponding thiosulfonates in the presence of water. The reaction proceeded smoothly through a radical process. On the other hand, the reaction using aliphatic thiols was necessary for the addition of iodide ions. Furthermore, disulfides were available in the procedure. The procedure could carry out under mild conditions. The cross ‐coupling of 4‐toluenethiol with 1‐butanethiol could give the corresponding unsymmetrical disulfide in good yield.