Convenient Preparation of 2,4‐Dithiapentane, Dimethyl Disulfide, and the Corresponding Deuterated Products from DMSO or [2H6]‐DMSO/(COCl)2

Abstract It has been found that 2,4‐dithiapentane and dimethyl disulfide are readily prepared in useful yields from DMSO/(COCl) 2 under different conditions. The reaction mixture of DMSO/(COCl) 2 was treated with 1 equivalent of Et 3 N and 15 equivalents of H 2 O to afford 2,4‐dithiapentane, whereas dimethyl disulfide was obtained by the treatment DMSO/(COCl) 2 with 10 equivalents of H 2 O without Et 3 N. The corresponding deuterated products, [ 2 H 8 ]‐2,4‐dithiapentane, [ 2 H 6 ]‐dimethyl disulfide, and [ 2 H 6 ]‐methyl methanethiosulfonate were also prepared from the reactions of [ 2 H 6 ]‐DMSO with (COCl) 2 .