in neat (no solvent) exclusion of moisture; condensation of F-compd. and Si-compd. in NMR-tube (-80°C), shaking, warming (-40°C), warming (2 h, -10°C), warming (5 h, 20°C); not isolated; (1)H-NMR-spctroscopy;
参考文献
Haas, Alois; Wingender, Norbert
Zeitschrift fuer Anorganische und Allgemeine Chemie, 1989 , vol. 576, p. 151 - 159
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
Padma, D. K.; Kumar, H. P. Sampath
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, 1992 , vol. 22, p. 1533 - 1550