The transformation of a large‐volume industrial by‐product and stable greenhouse gas fluoroform (HCF3) to useful products has recently received significant attention. Now, a simple and scalable preparation of AgCF3 by treatment of HCF3 with t‐BuOK and AgOAc is disclosed. The reactivity of the HCF3‐derived AgCF3 has been demonstrated by hydrotrifluoromethylation of alkenes and C−H trifluoromethylation of (hetero)arenes. This work not only provides a new avenue for the utilization of HCF3, but also presents a reliable and easy‐to‐execute synthesis of the relatively stable AgCF3 solution.
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