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Ytterbium perfluorooctanesulfonate [Yb(OPf)3] and perfluorooctanesulfonic acid [PfOH] catalyze the highly efficient dinitration of toluene, benzene, benzyl chloride, and chlorobenzene in fluorous media. Notably the process produces almost no waste acid, as opposed to the traditional case. The fluorous phase‐containing catalyst could be easily and efficiently recovered for reuse by simple phase separation.
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