in neat (no solvent) react. of SO3-vapor with KBF4 (dried at 200°C, finely powdered) at about 35°C, evaporation of an excess of SO3, solidifying of KBF4*4SO3, decompn. at 80°C, heating for 2.5 hours to 120 up to 130°C;;
in neat (no solvent) stirring complex salt in flask; evacuation; introduction of SO3 vapour in stages; keeping reactants in contact for 15-20 mins after addn. of last aliquot of SO3; cooling with liquid N2, then with alcohol bath at -50°C; apparatus described;; warming to room temp.; evacuation for about 6 h; filling with dry N2; repeated washing of solid fluorosulphate with dry ether; drying under vac.; detn. by IR, 19F-NMR; elem. anal.;;
参考文献
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, , vol. 22, p. 1533 - 1550