Reduction of ruthenium trichloride in DMSO; ruthenium dichloride DMSO Adduct
Submitted Jun 03, 2008, published Jun 03, 2008
DMSO (Fisher Scientific).
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%.
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.
Evans, Spencer and Wilkinson, J. Chem. Soc., Dalton Trans., 1973, 204
Duliere, Devillers and Marchand-Brynaert, Organometallics, 2003, 22, 804.
Keywords: Ruthenium, DMSO, Chloride, Ruthenium(II) starting material, reduction, inorganic compounds