Abstract Selective desulfurization of 2-alkyl-1, 3-dithianes,-oxathiolanes, or-thiazolidines 1 with one equivalent of tri-n-butyltin hydride yields acyclic compounds R 1 R 2 CHX (CH 2) n SSnBu 3 (X= S, O, NH; n= 2, 3),(2) which can be destannylated to the corresponding mercaptans 3.