Sulfur tetrafluoride → HCID 54089403, compound

Temperature

-70 °C

A solution of 10.5 g (0.043 mol) of lithium 2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethoxide in 60 ml of dibutyl ether was added dropwise to a solution of 8 ml (measured at -78° C., 0.15 mol) of sulfur tetrafluoride in 50 ml of dibutyl ether cooled to -70° C. The reaction mixture was warmed to 25° C., and the volatiles were distilled out at reduced pressure and condensed in a cold trap at -78° C. The condensate was fractionated to give (A) 2.91 g of 2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethoxysulfur trifluoride as a colorless liquid: bp 56° to 60°; 19F NMR (CCl3F) δ -71.4 ppm (q, J=3.0 Hz,9F) and 44.0 ppm (broad, 3F) and (B) 3.60 g of bis[2,2,2-trifluoro-1,1-(trifluoromethyl)ethoxy]sulfur difluoride as a colorless liquid: bp 35° to 37° C. (20 mm); 19F NMR (CCl3F) δ -71.7 ppm (t, J=1.5 Hz, 18F) and +32.1 ppm (broad, 2F).

1. temperatureThe reaction mixture was warmed to 25° C.
2. distillationthe volatiles were distilled out at reduced pressure and condensed in a cold trap at -78° C

ORD record

ord-69da4c8d076e4c6794e377dedde92f4b

Source dataset

uspto-grants-1983_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04382891