in hexane byproducts: SO2; Sonication; (Ar) VOCl3 in hexane at room temp. was added to soiln. t-BuNSO in hexane, refluxed for 2 h; volatiles were removed in vacuo at 20°C, residue was suspnd. in pentane by sonication and kept at -80°C for 24 h, ppt. was decanted, washed with chilled pentane and dried in vacuo;

in pentane byproducts: H2O; under Ar; slow addn. of amine soln. to dissolved VOCl3 under stirring at -78°C; stirred for 30 min; removing of ice bath; further stirring until reaction mixture was warmed up to 25°C; filtration of (NH3-t-bu-(VOCl3)2O); washed (CH2Cl2 and n-pentane); dried under vac.; solvent removed from mother liquor under vacuo; sublimation of residue (80°C, high vac.); elem. anal.; NMR; IR;

in hexane under N2; VOCl3 is added dropwise to a soln. of the starting complex inhexane at 0°C with stirring, cooled to -80°C, allowed to stand for 1 h; the solvent is decanted, the residue is washed, recrystd., elem. anal.;

in neat (no solvent) byproducts: Me3SiCl; under Ar; t-Bu-NVCl2(OSiMe3) heated at 120°C and 0.01 Torr under stirring for 3 h; sepn. by fractionated condensation (liquid N2); residue was stirred (n-pentane) at 25°C for 40 min; filtration; washed (n-pentane); dried under vacuum; elem. anal.; NMR;

in neat (no solvent) room temp. or sublimation (vac., 120°C);

in benzene under N2, stirred under reflux for 2 h; taken to dryness, filtered, washed with Et2O, dried under vac.; elem. anal.;