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Reduction of ruthenium trichloride in DMSO

SyntheticPage 274

Submitted: June 3, 2008, published: June 3, 2008

Authors

Suzanne Elizabeth Howson (s.e.howson@warwick.ac.uk)

A contribution from 

Reaction Scheme

Chemicals

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 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.

Keywords