A facile one‐pot gram‐scale synthesis of tetraalkylammonium tetrafluoridochlorate(III) [cat][ClF4] ([cat]=[NEt3Me]+, [NEt4]+) is described. An acetonitrile solution of the corresponding alkylammonium chloride salt is fluorinated with diluted fluor...
A facile one‐pot gram‐scale synthesis of tetraalkylammonium tetrafluoridochlorate(III) [cat][ClF4] ([cat]=[NEt3Me]+, [NEt4]+) is described. An acetonitrile solution of the corresponding alkylammonium chloride salt is fluorinated with diluted fluorine at low temperatures. The reaction proceeds via the [ClF2]− anion which is structurally characterized for the first time. The potential application of [ClF4]− salts as fluorinating agents is evaluated by the reaction with diphenyl disulfide, Ph2S2, to pentafluorosulfanyl benzene, PhSF5. The CN moieties in acetonitrile and [B(CN)4]− are transferred in CF3 groups. Exposure of carbon monoxide, CO, leads to the formation of carbonyl fluoride, COF2, and elemental gold is dissolved under the formation of tetrafluoridoaurate [AuF4]−.
The synthesis of tetraalkylammonium tetrafluoridochlorate(III) is described. An acetonitrile solution of the alkylammonium chloride salt is reacted with diluted fluorine at low temperature. The application as fluorinating agent is evaluated by the reaction with Ph2S2 to PhSF5, the transformation of the CN moieties in acetonitrile and [B(CN)4]− into CF3, reaction with CO to COF2 and the formation of tetrafluoridoaurate [AuF4]− with elemental gold.