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0.25 g of metal sodium was mixed with well dried tetrahydrofuran in a 100 ml flask whose inside had been substituted by nitrogen and cooled to -78 C. A solution of 1.3 g of trimethylsilyl cyclopentadiene dissolved in 30 ml of tetrahydrofuran was added dropwise to the above solution in a stream of nitrogen over 1 hour and heated to room temperature under agitation over 3 hours to obtain a tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium. Separately, 18 ml of a tetrahydrofuran solution (2.0 mol/l) of cyclopentadienyl sodium was prepared. Further separately, 5 g of dichloro(1,5-cyclooctadienyl)ruthenium was dissolved in 200 ml of well dried tetrahydrofuran in a 500 ml flask whose inside had been substituted by nitrogen. This solution was cooled to -78 C., and the above tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium and the above tetrahydrofuran solution of cyclopentadienyl sodium were added dropwise to the solution at the same time in a stream of nitrogen over 1 hour. The resulting solution was stirred at -78 C. for 3 hours and heated to room temperature under agitation over 12 hours. After the resulting solution was let pass through a neutral alumina column in an argon gas atmosphere to be purified and concentrated, it was separated and purified by a neutral alumina column again to obtain 0.23 g of trimethylsilyl cyclopentadienyl(cyclopentadienyl)ruthenium (yield rate of 4.3%).
bis(η5-(trimethylsilyl)cyclopentadienyl)ruthenium(II)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In tetrahydrofuran; at -78 - 20℃; for 16h;
11 g of trimethylsilyl chloride was dissolved in 30 mol of well dried tetrahydrofuran in a 300 ml flask whose inside had been substituted by nitrogen, and the obtained solution was cooled to -78 C. 100 ml of a tetrahydrofuran solution (2.0 mol/l) of cyclopentadienyl sodium was added dropwise to the above solution in a stream of nitrogen over 1 hour. The solution was stirred at -78 C. for 1 hour and returned to room temperature over 6 hours. A salt precipitated in the mixture solution was removed by filtration in a nitrogen atmosphere, and the residual solution was distilled to obtain 8 g of trimethylsilyl cyclopentadiene. 0.5 g of metal sodium was mixed with a well dried tetrahydrofuran solution in a 300 ml flask whose inside had been substituted by nitrogen, and the resulting solution was cooled to -78 C. A solution of 2.5 g of the above synthesized trimethylsilyl cyclopentadiene dissolved in 30 ml of tetrahydrofuran was added dropwise to the above solution in a stream of nitrogen over 1 hour and further heated to room temperature under agitation for 3 hours to obtain a tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium. Separately, 5 g of dichloro(cyclooctadienyl)ruthenium was dissolved in 200 ml of well dried tetrahydrofuran in a 500 ml flask whose inside had been substituted by nitrogen. This solution was cooled to -78 C., and the above synthesized tetrahydrofuran solution of trimethylsilyl cyclopentadienyl sodium was added dropwise to the above solution in a stream of nitrogen over 1 hour. The resulting solution was stirred at -78 C. for 3 hours and returned to room temperature under agitation over 12 hours. After the solution was let pass through a neutral alumina column in an argon gas atmosphere to be purified and concentrated, it was separated and purified by a neutral alumina column again to obtain 0.9 g of bis(trimethylsilylcyclopentadienyl)ruthenium (yield rate of 13%).
bis(trifluoromethylcyclopentadienyl)ruthenium[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
30%
In tetrahydrofuran; at -78 - 20℃; for 16h;
Separately, 200 ml of well dried tetrahydrofuran was fed to a 500 ml flask whose inside had been substituted by argon, and 5 g of dichloro(cyclooctadienyl)ruthenium was injected into the flask and well mixed with the above tetrahydrofuran to obtain a suspension. This suspension was cooled to -78 C. in a stream of argon, and 15 ml of the above synthesized tetrahydrofuran solution of trifluoromethyl cyclopentadienyl sodium was added dropwise to the suspension over 1 hour. The reaction mixture was further stirred at -78 C. for 3 hours and returned to room temperature under agitation over 12 hours. After the reaction mixture was let pass through a neutral alumina column in a stream of argon to be purified and concentrated, it was purified again by a neutral alumina column to obtain 0.2 g of bis(trifluoromethylcyclopentadienyl)ruthenium (yield rate of 30%).
Separately, 200 ml of well dried tetrahydrofuran was fed to a 500 ml flask whose inside had been substituted by argon, and 5 g of dichloro(cyclooctadienyl)ruthenium was injected into the flask and well mixed with tetrahydrofuran to obtain a suspension. This suspension was cooled to -78 C. in a stream of argon, and 14 ml of a tetrahydrofuran solution of the above synthesized fluorocyclopentadienyl sodium was added dropwise to the above suspension over 1 hour. The obtained reaction mixture was further stirred at -78 C. for 3 hours and returned to room temperature under agitation over 12 hours. After the reaction mixture was let pass through a neutral alumina column in a stream of argon to be purified and concentrated, it was purified again by a neutral alumina column to obtain 0.4 g of bis(fluorocyclopentadienyl)ruthenium (yield rate of 8.4%).
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