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Reduction of ruthenium trichloride in DMSO; ruthenium dichloride DMSO Adduct

SyntheticPage 274
DOI: 10.1039/SP274
Submitted Jun 03, 2008, published Jun 03, 2008
Suzanne Elizabeth Howson (s.e.howson@warwick.ac.uk)
A contribution from Scott group, Warwick University


			Reaction Scheme: Reduction of ruthenium trichloride in DMSO

Chemicals Used

RuCl3 (Johnson-Matthey),
DMSO (Fisher Scientific).

Procedure

Ruthenium trichloride (6.00 g, 28.9 mmol) was refluxed in DMSO (30 ml) for 5 minutes before cooling to ambient temperature. Acetone (50 ml) was added and the solution poured into a crystallising dish. After 3 days the orange crystals formed were filtered, washed with acetone (20 ml) and diethyl ether (20 ml). Recrystallisation from hot DMSO yielded yellow crystals, which were filtered, washed with acetone (20 ml) and diethyl ether (20 ml), and dried in the vacuum oven (50oC) overnight. Yield = 7.52 g, 15.5 mmol, 54%.

Author's Comments

The filtrate was left to stand and allowed further product to be collected.

Data

1H NMR (400 MHz, 298 K, CDCl3) 3.53, 3.50, 3.43, 3.33 (Me of DMSO, S-Ru linked), 2.73 (Me of DMSO, O-Ru linked), 2.61 (Me of free DMSO). Ratio S-Ru:O-Ru 4:1.

Lead Reference

Evans, Spencer and Wilkinson, J. Chem. Soc., Dalton Trans., 1973, 204

Other References

Duliere, Devillers and Marchand-Brynaert, Organometallics, 2003, 22, 804.

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Keywords: Ruthenium, DMSO, Chloride, Ruthenium(II) starting material, reduction, inorganic compounds

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