Trifluoromethylthiocopper can be prepared using two different procedures (eq 1). Heating of finely divided Copper powder with bis(trifluoromethylthio)mercury neat at 80-100 °C until the appearance of an orange color persists, and then heating for 30 min at 150 °C, gives the desired product upon cooling, ether extraction, and evaporation. Stirring copper powder and bis(trifluoromethyl) disulfide in DMF for 1 h gives trifluoromethylthiocopper as its 1:1 DMF adduct. Additionally, this reagent has been prepared by metal exchange of trifluoromethylthiosilver with Copper(I) Bromide.