Vanadium Carbonyl - Synthesis

Synthesis

Traditionally V(CO)6 is prepared in two-steps via the intermediacy of −. In the first step, VCl3 is reduced with metallic sodium under 200 atm CO at 160 °C. The solvent for this reduction is typically diglyme, CH3OCH2CH2OCH2CH2OCH3. This triether solubilizes sodium salts, akin to the behavior of a crown ether:

4 Na + VCl3 + 6 CO + 2 diglyme → + 3 NaCl

The resulting anion is oxidized with acid:

2 - + H3PO4 → 2 V(CO)6 + H2 + 2 H2PO4-

An improved low pressure synthesis has been developed.

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