in neat (no solvent) The reactor with SF3N and ClF was warmed from -196°C to -78°C over 14 h; addn. of F2, warming; pumped through traps at -78, -115, and -196°C;
in neat (no solvent) heating in cooled copper tube (water) to 650°C; description of apparatus given;; condensed (liquid O2); passed through flasks containing H2O and hot aq. KOH; dried over P2O5;;
参考文献
S: MVol.B3, 83, page 1712 - 1714
Brauer, G., Handbuch der praeparativen anorganischen Chemie, 2. Aufl., Bd. 1, Stuttgart 1960, S. 166
Brauer, G., Handbuch der praeparativen anorganischen Chemie, Stuttgart 1954, S. 140
in neat (no solvent) byproducts: OF2; introduction of F2 into steel chamber, sulfur in compartments; detailed description of apparatus and handling given;; first passing through Ni (or Monel) tube (400°C); second Cu column (H2O sprayed); passed into steel column (containing carbon/Fe shavings; aq. NaOH sprayed); dried in column (containing solid NaOH, BaO or P2O5);;
参考文献
Industrial and Engineering Chemistry, , vol. 39, p. 421 - 423
S: MVol.B3, 83, page 1712 - 1714
Inorganic syntheses, Bd. 3, New York 1950, S. 119/123
SiO2 in neat (no solvent, gas phase) introduction of F2 stream into liquid SOF2 (-50°C); mixture (F2/SOF2) escapes into quartz tube (containing heated Pt net/150°C); pale red flame observed; abs. exclusion of air;; condensed (liquid air cooling); removal of F2 (water jet pump/-190°C); fractionated (quartz column);;
disulfonyl fluoride in not given SO2F2 and F2 were added to S2NAsF6 at -196°C, mixt. was stirred for 4 h while held at -78°C, mixt. was stirred at room temp. for 20h; volatiles were removed, products were not isolated; products were analized by IR;
参考文献
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), , p. 1961 - 1968