a) Preparation of [RuI2p-isocumene]2: Under nitrogen atmosphere, 2 g of [RuCI2p-isocumene]2 and 50 mL of dichloromethane were placed in a flask. 66 mg of tetramethylammonium iodide and subsequently 50 mL of an aqueous solution containing 10.2 mg of KI were added to the solution. The mixture was vigorously stirred at room temperature under an inert atmosphere for about 15 hours to separate the phases.
The aqueous phase was extracted with 2×40 mL of dichloromethane, and the combined organic phases were washed with 3×40 mL of water, dried over sodium sulfate, and filtered through a decalitator. A reddish-brown solution was obtained, which was dried under vacuum to give 3.07 g of [RuI
2p-isopropylphenyl]
2.
b) Preparation of diiodo(p-cymene)ruthenium(II) dimer: 155 mg of [RuI2p-isopropylphenyl]2 and 204 mg of (+)TMBPT were placed in a flask under nitrogen atmosphere, and a mixture of 80 mL of dichloromethane and 30 mL of nitrogen-degassed methanol was added. The mixture was stirred under reflux for 1.5 h, then cooled and concentrated under reduced pressure to obtain the desired product.
