Oxidation of iron metal with nitrosyl tetrafluoroborate; [Fe(MeCN)6][BF4]2
SyntheticPage 665
DOI:
10.1039/SP665
Submitted Jul 26, 2013, published Jul 29, 2013
Chemicals Used
Iron powder (Aldrich)
Nitrosyl tetrafluoroborate (Aldrich)
Acetonitrile (distilled over calcium hydride)
Procedure
A Schlenk flask was charged with iron powder (189 mg, 3.38 mmol) and nitrosyl tetrafluoroborate (790 mg, 6.76 mmol), the vessel was cooled to -78°C and dry acetonitrile (30 cm3) was added. The suspension was left to warm to ambient temperature and left to stir for 12 h. The resulting golden solution was filtered to remove any unreacted iron and insoluble materials and concentrated in vacuo to ca.10 cm3. The compound crystallised out upon layering with diethyl ether (20 cm3), isolated by filtration and dried in vacuo for 2 h. The solid was stored in the inert gas dry box thereafter. (1.38 g, 86%)
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.
A convenient synthesis of a water-free soluble source of Fe(II)
Data
IR (cm-1): 2285, 2308, 1634, 1305, 1128, 1035, 945, 765
Melting point: 116-117 °C (Lit value: 114-116 °C)
Fe by ICP: 11.71 (11.74)%.
Lead Reference
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, inorganic compounds, iron powder, oxidation, substitution, tetrafluoroborate
