1) Dehydration of cobalt (II) tetrafluoroborate

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Published Jul 29, 2013

Reaction Scheme

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%).

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2) Oxidation of iron metal with nitrosyl tetrafluoroborate

SyntheticPage 665
Published Jul 29, 2013

Reaction Scheme

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%)

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