To produce the subject compound having low metal-corrosive property and useful as an antioxidant for a lubricating oil, an insecticide or the like in high yield under mild conditions by subjecting a mercaptan to catalytic reaction with sulfur in the presence of a base catalyst, and allowing the obtained reaction medium to come in contact with an acid.
In the presence of (A) a base catalyst such as tetramethylammonium hydroxide, sodium hydroxide or sodium phenoxide, (B) a mercaptan (e.g. t-butyl mercaptan) is subjected to catalytic reaction with (C) elemental sulfur, and the obtained reaction medium is allowed to come in contact with (D) an acid such as sulfuric acid, phosphoric acid or p- toluenesulfonic acid to obtain the objective compound (e.g. t-butyl trisulfide).