A new synthetic protocol to give a variety of symmetric diaryl disulfides from odorless and easily available phenyl dimethylcarbamodithioates was developed. By using phenyl dimethylcarbamodithioates as organosulfur source, the target products were furnished smoothly through simple hydrolysis, giving a series of symmetric diaryl disulfides. The protocol features simple operation, odorless and easily available organosulfur source and high yield.