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We report herein a practical approach for synthesis of an electrophilic trifluoroethylthiolation reagent PhS02SCH2CF3(1)from easily available materials.The reaction proceeded through a protonation and nucleophilic substitution cascade of the in situ formed trifluorodiazoethane.This bench-stable reagent could easily be applied to introduce trifluoroethylthio group into small organic molecules.