As a model study, a series of linear and branched p-phenylene and m-phenylene sulfides, functionalized by a thiomethyl group, were deprotected to thiols while using various alkyl thiolates at 160° C in DMF. Many complex aromatic thiols were obtained in almost quantitative yields from a trivial purification and without significant contamination by disulfides. This methodology is reliable, efficient and has been optimized on several ...