Since the SS bond of polysulfides plays a vital role in biological processes, the chemistry of the SS bond has attracted considerable attention. The reaction of bis-(trifluoromethyl) trisulfide with organolithium reagents at −78 °C has now been found to cause simultaneous scissions of the CS and SS bonds and to furnish mixed monosulfides, disulfides and trisulfides containing the trifluoromethyl