Methods of synthesizing ruthenium and osmium compounds
A technology of compounds and ruthenium complexes, applied in the directions of osmium organic compounds, ruthenium organic compounds, phosphorus organic compounds, etc., can solve problems such as long reaction time, no teaching or suggestion of reaction route, etc.
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Embodiment 1
[0019] Preferred embodiments of the invention are described herein.
[0020] Will Ru 3 (CO) 12(2.0 g, 3.13 mMol) was transferred to a dry 25 ml round bottom flask equipped with a water condenser and a Teflon-coated magnetic stir bar. 1,3-Cyclohexadiene (5 ml, 52.5 mMol, greater than 5-fold excess) was added using a syringe. Under a dry nitrogen atmosphere, the mixture was heated to reflux with stirring for 5 hours to obtain a clear yellow solution. Heating was stopped to allow the mixture to cool to room temperature. Excess 1,3-cyclohexadiene was removed using rotary evaporation. Under the pressure of 0.1 torr, carry out vacuum distillation to obtain 1,3-cyclohexadienetricarbonyl ruthenium (C 6 h 8 )Ru(CO) 3 (2.1 g, 7.92 mMol, 84% yield).
[0021] Using GC-MS, 1 H NMR, 13 C NMR, FTIR, and ICP-MS (metal content) to characterize the compound. The obtained analysis data ( 1 H& 13 C NMR) consistent with literature values for this compound. Figures 1, 2 and 3 show t...
Embodiment 2
[0023] This is another example where it is expected that triosmium dodecacarbonyl (Os 3 CO 12 ) and 1,3-cyclohexadiene generate 1,3-cyclohexadiene tricarbonyl osmium (C 6 h 8 )Os(CO) 3 . This reaction was carried out under the same conditions as in Example 1 above. 2gOs 3 (CO) 12 (2.2mMol) into the flask. Then about 5 ml of 1,3-cyclohexadiene (52.5 mMol, >5-fold excess) was added and the mixture was refluxed for several hours. The substitution of osmium for ruthenium proceeded in similar yields, physical properties and reactivity. This is consistent with the generally accepted periodic nature of the elements.
[0024] The present invention's most preferred preparation process step of ruthenium and osmium compound is as follows:
Embodiment 3
[0026] 87.26g (0.136Mol) Ru 3 (CO) 12 Place into a 3-neck RB flask equipped with a Teflon-coated magnetic stir bar, condenser, and gas stopcock. Add 220ml (185g, 2.31mol) C 6 h 8 . The device was flushed with nitrogen and then kept under nitrogen for the remainder of the process. The mixture was heated to gentle reflux and stirred for 44 hours, at which point it was a cloudy yellow / orange mixture. At 80 °C, under atmospheric pressure, the mixture yielded 120 ml of unreacted C 6 h 8 . Vacuum distillation (at P = 0.1 Torr) of the remaining mixture yielded 103.32 g (C 6 h 8 )Ru(CO) 3 (0.39 mol, 95% yield) (>99.8% by GC-MS).
[0027] Excess ligand was removed by distillation. The refluxed reaction mixture was subjected to rotary evaporation at ≈10 Torr and 60 °C, due to the 1,3-C 6 h 8 A lower relative vapor pressure, such that removal of excess of the species removes non-reactive solvent and excess ligand. Finally, the resulting refluxed reaction mixture from which...
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