Kinetics; byproducts: Cl2;

in neat (no solvent) ClOSO2F trasferred under vac. to FEP reactor fitted with stainless-steel valve and held at -196°C, SF4 condensed, reactor placed in bath at -90°C and allowed to warm to -40°C for 4 h; reactor cooled to -70°C, volatile materials(SF5Cl) removed, reactor warmed to -40°C and then - to 23°C and held under dynamic vac. for 10 min;

SbF5 in epoxysulfonyl fluoride byproducts: CF2O; bubbling CF2Cl2 through a mixt. of ClOSO2F, SbF5, and HSO3F, <=40°C, 2 h;

SbF5 in epoxysulfonyl fluoride byproducts: fluorosulfonyloxydifluoroacetyl fluoride; dropwise addn. of CF2ClCFCl2 to a mixt. of ClOSO2F, SbF5, and HSO3F, stirring, <=30°C; fractionation;

in neat (no solvent) ClOSO2F transferred under static vac. to FEP reactor, SF4 condensed andreactor placed in 0°C bath and left for 1.5 h; reactor cooled to -95°C, volatile materials pumped from -95 to -70°C, reactor allowed to warm to room temp., volatile materials pumped into -196°C trap and fractionated, product refractionated through -63°C trap;