sodium chloride in dichloromethane distn. of a react.-mixt. of urea and HSO3F under vac.; distillate dissolved in CH2Cl2; NaCl added; stirred for 6 h under reflux;; NaSO3F filtered off; filtrate cooled to -80°C; filtn., recrystn. (CFCl3, -80°C).;

2oo ° C, N2 stream;

in neat (no solvent) mixed in Pt retort (reflux cooler/vigorous evolution of HCl vapour); then heating for 0.5h (230°C);;

sulfur dioxide over 150°C;

in 2-methyl cyclohexane N2 atm.; cooling (1 h, -78°C), stirring (room temp., 72 h); evapn. (1E-4 torr), extraction (pentane, toluene (25°C, 20 torr)), acetonitrile (30°C, 50 torr)), concn., crystn. (-20°C);

in neat (no solvent) vigorous evolution of HF;;

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.;;

calculated amts. of NaF added with care; heating of mixture to 250°C (melting); cooling down; reducing to small peaces; soluting in a small amts. of water; neutralisation with NaOH; evapn. in vac. over H2SO4 absolutely; residue extracted by hot methanol; evapg. by warm air stream; recrystd. from a little amts. of methanol;

in 2-methyl cyclohexane N2 atm.; cooling (1 h, -78°C), stirring (room temp., 72 h); extraction (toluene (30°C, 30 torr), acetonitrile (vac.)), concn.(0.05 torr, 25°C), centrifugation, crystn. (PhMe/CH3CN, 10/1-1/3 );

in acetonitrile N2 atm.; cooling (-78°C), heating (30 min, -40°C), stirring (2 h); extraction (pentane, toluene), dissoln. (CH3CN), centrifugation, addn. of toluene; elem. anal.;