Reduction of ruthenium trichloride in DMSO; ruthenium dichloride DMSO Adduct
SyntheticPage 274
DOI:
10.1039/SP274
Submitted Jun 03, 2008, published Jun 03, 2008
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