Patent US6576778B1 successfully refreshed from Google Patents.
US6576778B1
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Methods for preparing ruthenium and osmium compounds
Assignee: Micron Technology Inc
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Filing: 2000-08-29
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Granted: 2003-06-10
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Expires: 2020-08-29
Abstract
Abstract The present invention provides methods for the preparation of compounds of the formula (Formula I):wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5. These methods involve the reaction of Ru3(CO)12 or Os3(CO)12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure.
Inventors
- 👤 Stefan Uhlenbrock
- 👤 Brian A. Vaartstra
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 02:21
CPC Classifications
C; C07; C07F; C07F15/00; C07F17/00; C07F17/02; C07F15/0006; C07F15/002; C07F15/0026; C07F15/0046; C07F15/0053
Claims Analysis
Total Claims: 37
Claim 1
Independent Claim
80 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or OS, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein a complex of Formula I is prepared in an amount of greater than about 99%.
Claim 2
Independent Claim
80 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or OS, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein a complex of Formula I is prepared in an amount of greater than about 99%.
Claim 3
Dependent Claim
13 words
The method of claim 1 wherein the solvent system comprises only one solvent.
Claim 4
Dependent Claim
14 words
The method of claim 1 wherein the solvent system comprises two or more solvents.
Claim 5
Dependent Claim
57 words
The method of claim 1 wherein the solvent system comprises a solvent selected from the group of saturated or unsaturated hydrocarbons, aromatic hydrocarbons, halogenated hydrocarbons, silylated hydrocarbons, ethers, polyethers, thioethers, esters, lactones, amides, amines, polyamines, nitrites, cyanates, isocyanates, thiocyanates, silicone oils, aldehydes, ketones, diketones, carboxylic acids, alcohols, thiols, and mixtures of one or more of the above.
Claim 6
Dependent Claim
29 words
The method of claim 4 wherein the solvent system comprises at least one solvent selected from the group of toluene, xylene, substituted benzene, heptane, octane, nonane, and combinations thereof.
Claim 7
Dependent Claim
55 words
The method of claim 1 wherein each L is independently selected from the group of phosphines, phosphites, amines, arsines, stibenes, ethers, sulfides, alkylidenes, nitrites, isonitriles, thiocarbonyls, linear, branched, or cyclic monoalkenes, linear, branched, or cyclic, dienes, linear, branched, or cyclic trienes, bicyclic alkenes, bicyclic dienes, bicyclic trienes, tricyclic alkenes, tricyclic dienes, tricyclic trienes, and alkynes.
Claim 8
Dependent Claim
25 words
The method of claim 6 wherein L is selected from the group of linear, branched, or cyclic dienes, bicyclic dienes, tricyclic dienes, and combinations thereof.
Claim 9
Independent Claim
106 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein the solvent system comprises at least one solvent selected from the group of toluene, xylene, substituted benzene, heptane, octane, nionane, and combinations thereof; and further wherein a complex of Formula I is prepared in an amount of greater than about 95%.
Claim 10
Independent Claim
106 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein the solvent system comprises at least one solvent selected from the group of toluene, xylene, substituted benzene, heptane, octane, nionane, and combinations thereof; and further wherein a complex of Formula I is prepared in an amount of greater than about 95%.
Claim 11
Independent Claim
113 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein the solvent system comprises at least one solvent selected from the group of toluene, xylene, substituted benzene, heptane, octane, nonane, and combinations thereof; and further wherein a complex of Formula I is prepared in an amount of greater than about 95% in no greater than about 36 hours.
Claim 12
Independent Claim
113 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein the solvent system comprises at least one solvent selected from the group of toluene, xylene, substituted benzene, heptane, octane, nonane, and combinations thereof; and further wherein a complex of Formula I is prepared in an amount of greater than about 95% in no greater than about 36 hours.
Claim 13
Independent Claim
87 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure wherein a complex of Formula I is prepared in an amount of greater than about 99% in no greater than about 24 hours.
Claim 14
Independent Claim
87 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure wherein a complex of Formula I is prepared in an amount of greater than about 99% in no greater than about 24 hours.
Claim 15
Independent Claim
85 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in an inert atmosphere with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure, and isolating the compound of Formula I by removing the solvent system and unreacted ligand in vacuo.
Claim 16
Independent Claim
85 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in an inert atmosphere with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure, and isolating the compound of Formula I by removing the solvent system and unreacted ligand in vacuo.
Claim 17
Independent Claim
106 words
A method for the preperation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z= 1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure, wherein the neutral ligand is present in an amount of at least about a 3-fold excess relative to Ru 3 (CO) 12 or Os 3 (CO) 12 , and further wherein the reaction is carried out in the presence of CO.
Claim 18
Independent Claim
106 words
A method for the preperation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z= 1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure, wherein the neutral ligand is present in an amount of at least about a 3-fold excess relative to Ru 3 (CO) 12 or Os 3 (CO) 12 , and further wherein the reaction is carried out in the presence of CO.
Claim 19
Independent Claim
79 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising: reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in an inert atmosphere with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure to provide a reaction mixture, and vacuum distilling the reaction mixture.
Claim 20
Independent Claim
79 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising: reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in an inert atmosphere with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure to provide a reaction mixture, and vacuum distilling the reaction mixture.
Claim 21
Dependent Claim
20 words
The method of claim 13 wherein the vacuum distillation is carried out at a pressure less than about 70 mTorr.
Claim 22
Dependent Claim
11 words
The method of claim 13 wherein the reaction mixture is heated.
Claim 23
Dependent Claim
17 words
The method of claim 13 wherein the reaction mixture is heated to at least about 35° C.
Claim 24
Dependent Claim
32 words
The method of claim 13 wherein the vacuum distillation is carried out at a pressure less than about 70 mTorr and the reaction mixture is heated to at least about 35° C.
Claim 25
Dependent Claim
57 words
The method of claim 13 wherein the solvent system comprises a solvent selected from the group of saturated or unsaturated hydrocarbons, aromatic hydrocarbons, halogenated hydrocarbons, silylated hydrocarbons, ethers, polyethers, thioethers, esters, lactones, amides, amines, polyamines, nitrites, cyanates, isocyanates, thiocyanates, silicone oils, aldehydes, ketones, diketones, carboxylic acids, alcohols, thiols, and mixtures of one or more of the above.
Claim 26
Dependent Claim
29 words
The method of claim 18 wherein the solvent system comprises at least one solvent selected from the group of toluene, xylene, substituted benzene, heptane, octane, nonane, and combinations thereof.
Claim 27
Independent Claim
98 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising: reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure to provide a reaction mixture; and vacuum distilling the reaction mixture; wherein a complex of Formula I is prepared in an amount of greater than about 95% in no greater than about 24 hours.
Claim 28
Independent Claim
98 words
A method for the preparation of a complex of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising: reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure to provide a reaction mixture; and vacuum distilling the reaction mixture; wherein a complex of Formula I is prepared in an amount of greater than about 95% in no greater than about 24 hours.
Claim 29
Dependent Claim
55 words
The method of claim 13 wherein each L is independently selected from the group of phosphines, phosphites, amines, arsines, stibenes, ethers, sulfides, alkylidenes, nitrites, isonitriles, thiocarbonyls, linear, branched, or cyclic monoalkenes, linear, branched, or cyclic dienes, linear, branched, or cyclic trienes, bicyclic alkenes, bicyclic dienes, bicyclic trienes, tricyclic alkenes, tricyclic dienes, tricyclic trienes, and alkynes.
Claim 30
Dependent Claim
25 words
The method of claim 21 wherein L is selected from the group of linear, branched, or cyclic dienes, bicyclic dienes, tricyclic dienes, and combinations thereof.
Claim 31
Dependent Claim
33 words
The method of claim 13 wherein the neutral ligand is present in an amount of up to about a 20-fold excess relative to Ru 3 (CO) 12 or Os 3 (CO) 12 .
Claim 32
Independent Claim
86 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising: reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure to provide a reaction mixture; and vacuum distilling the reaction mixture; wherein the reaction is carried out in the presence of CO.
Claim 33
Independent Claim
86 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising: reacting Ru 3 (CO) 12 or Os 3 (CO) 12 with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure to provide a reaction mixture; and vacuum distilling the reaction mixture; wherein the reaction is carried out in the presence of CO.
Claim 34
Independent Claim
96 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in an inert atmosphere with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein the neutral ligand is present in an amount of up to about a 20-fold excess relative to Ru 3 (CO) 12 or Os 3 (CO) 12 .
Claim 35
Independent Claim
96 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in an inert atmosphere with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure; wherein the neutral ligand is present in an amount of up to about a 20-fold excess relative to Ru 3 (CO) 12 or Os 3 (CO) 12 .
Claim 36
Independent Claim
69 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in the presence of CO with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure.
Claim 37
Independent Claim
69 words
A method for the preparation of a compound of Formula I: L y M(CO) z wherein M is Ru or Os, each L is independently a neutral ligand, y=1-4, and z=1-5, the method comprising reacting Ru 3 (CO) 12 or Os 3 (CO) 12 in the presence of CO with a neutral ligand in a solvent system having a boiling point higher than that of benzene at atmospheric pressure.
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| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 2006-06-09 | 2006-12-09 | 2007-06-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2010-06-09 | 2010-12-09 | 2011-06-10 | $3760.00 | Window Closed / Lapsed |
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