in sulfur dioxide absence of air and moisture; condensing excess SO2 onto metal fluoride at -196°C, warming in sealed tube to room temp., stirring for 1 d; evapn. (pumping at dry-ice temp.); yield depending on source of KF;
in neat (no solvent) heating (NPCl2)3 with KSO2F at 120-140 °C; formation of a colorless mixt. of fluoride chlorides;; fractionation;;
参考文献
Chapman, A. C.; Paine, D. H.; Searle, H. T.; Smith, D. R.; White, R. F. M.
Journal of the Chemical Society, 1961 , p. 1768 - 1771
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Gmelin Handbook: P: MVol.C, 247, page 564 - 567
in neat (no solvent) refluxing PSCl3 with KSO2F in an atmosphere of N2; formation of two layers in the freezing trap;; the upper layer contains PSF3 and a small amount of PSF2Cl, the other SO2; isolation on distg. at ambient pressure in an atmosphere of N2, use of liquid air and dry ice as cooling agent;;
in nitrobenzene heating a soln. of (NPCl2)3 in C6H5NO2 with solid 90 percent KSO2F on refluxing; react. starting at 100. degree.C under evolution of gas;; condensation of (NPCl2)3 and formed SO2 on cooling with dry ice; isolation on distg. at 0 °C;;
in further solvent(s)
byproducts: SO2; react. of KSO2F with (Ni(PCl3)4) under exclusion of air and moisture in m-dichlorobenzene (cooling with ice), stirring for 30 min at ambient temp. and for 2 h at 90 °C;; collecting volatile react. products in cooled U-tube (filled with KSO2F), distilling into second U-tube after evapn. of SO2, distillation of (Ni(PF3)4) in micro-column at 760 torr under N2;;
in nitrobenzene
heating a soln. of (NPCl2)4 in C6H5NO2 with solid 90 percent KSO2F on refluxing; react. starting at 80. degree.C under evolution of gas;; condensation of (NPCl2)3 and formed SO2 on cooling with ice-water; distn. in vac.;;