Sauron - 20-8-2008 at 04:07
Here is a facile prep of vanadium tetrachloride (VCl4), vanadium oxychloride (VOCl3) and titanium tetrachloride (TiCl4) from trichoromethylbenzene.
I ran across this in the course of reading up on the preparation of a,a,a,a',a',a'-hexachloroxylenes (both m- and p-isomers) in connection with my
interest in their use to prepare non-metallic oxides such as SOCl2 and POCl3.
Titanium dioxide reacts with HCMX at 220-270 C and TiCl4 distills off, the isophthalyl or terephthalyl chloride remaining is then distilled in vacuo.
Yields of both are 95%.
Similarly V2O5 and HCMX gives VOCl3 while the commercially available benzotrichloride gives VCl4.
The metal oxides need to be very low in iron and aluminum.
See the attached communication from JACS.
[Edited on 20-8-2008 by Sauron]
Attachment: ja01546a076.pdf (253kB)
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