335-05-7

103 g (1.78 mol) of 1% aqueous potassium fluoride was fed into a 500 mL pressure-resistant reaction vessel, cooled to 5°C with ice water, and degassed under vacuum. 100 g (0.595 mol) of trifluoromethanesulfonyl chloride was added. The reactor was sealed and the temperature was slowly increased, and stirred for 4 hours at an internal temperature of 40–50°C. At this point, the reactor pressure was 0.94 MPa. The gas inside the reactor was circulated through a condenser cooled to -40°C to -20°C and collected using a liquid nitrogen-cooled trap. 80.3 g of the collected material was obtained. Gas chromatography (GC) analysis confirmed the formation of trifluoromethanesulfonyl fluoride, yielding a purity of 98.9% and a yield of 88% (99% conversion, 89% selectivity).