To a 150.0 mL 3-neck flask was added IrCl3·3H2O (1.0
g, 3.0 mmol) followed by addition of 95% of ethanol (17.0 mL), water (8.5 mL)
and 1,5-cyclooctadiene (3.0 mL, 24.5 mmol) under nitrogen atmosphere. The resulting
mixture was stirred under reflux for 24 h and formed a brick red precipitate.
It was allowed to cool to room temperature and filtered. The precipitate was
rinsed with cold methanol to remove the trace amount of 1,5-cyclooctadiene
unreacted. Then the product was dried in vacuum for 8 h. And [Ir(COD)Cl]2
was obtained in 67% yield as a brick red solid. mp 200–202 °C.
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