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New Developments in Superacid Chemistry: Characterization of HC+ =O and FC+ =O Cations.

A high gas pressure and use of the superacid HF/SbF5 (1/1) were required for direct spectroscopic characterization of the HC+ =O cation, which was until recently discussed as the short-lived intermediate of carbonylation reactions. The fluorocarbonyl cation FC+ =O, which was equally difficult to characterize, was also directly observed with NMR spectroscopy as the product of protolytic cleavage of tert-butyl fluoroformate [Eq. (a)].