Technology Process of (tert-butylimino)(trichloro)vanadium
There total 8 articles about (tert-butylimino)(trichloro)vanadium which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
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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;
DOI:10.1039/c0dt01133a
- Guidance literature:
-
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;
- Guidance literature:
-
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.;