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RSO2F (R = alkyl, cycloalkyl) were prepd. by the reaction of RSH or R2S2 with NO2 or N2O4 and HF. Thus, n-C8H17SH was emulsified with 83.3% HF, followed by the addn. of NO2 at 25 Deg to give 87% C8H17SO2F. [on SciFinder (R)]