VANADIUM(V) TRICHLORIDE OXIDE synthesis

Yield:-

Reaction Conditions:

at 80 - 128;

Steps:

Vanadium(V) oxytrichloride, VOCl3, was prepared by substantiallymodifying a published method [15]. 20.0 g (0.11 mol) ofvanadium pentoxide was boiled under reflux (cold finger condenserin a Claisen head) in 22.0 ml (0.30 mol) of thionyl chloride,protected from moisture in the air by granulated calcium chloride,for two hours at 80 C until the formation of the condensatestopped; then the temperature of the reaction mass was adjustedto 128 C, and it was boiled for another hour. Water was removedfrom the finger condenser and the required amount of the productwas distilled off at 126-127 C through a descending Liebig condenser.The ground glass joints were lubricated with fluorinatedgrease.

References:

Dzyuba, Valeriy I.;Koval, Lyudmila I.;Shtokvysh, Olherd O.;Trachevskii, Volodymyr V.;Pekhnyo, Vasyl I. [Polyhedron,2020,vol. 180,art. no. 114421]

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