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Dehydration of cobalt (II) tetrafluoroborate; [Co(MeCN)6][BF4]2

SyntheticPage 664
DOI: 10.1039/SP664
Submitted Jul 26, 2013, published Jul 29, 2013
Jan M. Becker (j.m.becker@warwick.ac.uk), Pratik Gurnani (pratik.gurnani@warwick.ac.uk)
A contribution from Scott group, Warwick University
Reaction Scheme: <IMG src="/images/empty.gif">Dehydration of <SPAN id=csm1375177017314 class=csm-chemical-name title="cobalt (II) tetrafluoroborate" grpid="2">cobalt (II) tetrafluoroborate</SPAN><IMG src="/images/empty.gif">

Chemicals Used

Hydrated cobalt (II) tetrafluoroborate (Aldrich)
Acetonitrile (distilled over calcium hydride)
Ethyl orthoformate (Fluka)

Procedure

Hydrated cobalt (II) tetrafluoroborate (10.21 g, 0.03 mmol) was dissolved in dry acetonitrile (13 cm3) and ethyl orthoformate (36.0 g, 0.24 mmol) was added. The resulting red solution was refluxed under argon for 1 h and all volatiles removed in vacuo. The orange solid was taken up in dry acetonitrile (15 cm3), layered with diethyl ether (20 cm3) and stored at 4°C overnight. The orange crystals formed were isolated by filtration and dried in vacuo for several hours. The compound was analysed by melting point and IR, which were found to be in good agreement with reported literature values. (9.62 g, 67%).

Author's Comments

Procedure was carried out under an inert atmosphere of argon by using a dual manifold vacuum/argon line and standard Schlenk techniques

Data

IR (cm-1): 2290, 2314, 1630, 1305, 1075, 1030, 943, 765

Melting point: 125-127°C (Lit. value: 127-130°C)

Co by ICP: 12.31 (12.35)%.

Lead Reference

van Leeuwen, P. W. N. M. and Groeneveld, W. L., Inorg. Nucl. Chem. Lett., 1967, 3, 145.
http://dx.doi.org/10.1016/0020-1650(67)80150-8

Other References

Hathaway, B. J., Holah, D. G. and Underhill, A. E., J. Chem. Soc., 1962, 2444.
http://dx.doi.org/10.1039/jr9620002444

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Keywords: acetonitrile, cobalt, hydrate, organometallics, substitution, tetrafluoroborate, water