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US4593113A
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Synthesis of transition metal dithiene complexes
Assignee: NAVY United States, AS REPRESENTED BY
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Filing: 1985-01-14
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Granted: 1986-06-03
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Expires: 2005-01-14
Abstract
Abstract The preparation of transition metal dithiene complexes is disclosed. By the process improved yields of the metal dithiene complexes are realized by substituting highly polar aprotic solvents such as N-methylpyrrolidinone or high boiling point solvents such as diethylene glycol in place of dioxane in the reaction sequence.
Inventors
- 👤 Martin H. Kauffman
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 23:07
CPC Classifications
C; C07; C07F; C07F15/00
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
90 words
A process for the synthesis of a transition metal dithiene complex comprising: a. reacting a dimethylaminobenzoin with a phosphorus sulfide and dioxane under suitable reaction conditions to produce a dioxane insoluble thiophosphoric ester derivative of the benzoin; b. adding excess dioxane and dissolving said thiophosphoric ester derivative in a highly polar aprotic solvent; c. reacting said ester derivative dissolved in said aprotic solvent with an aqueous solution of a reactive water soluble ionizable compound of a transition metal complex; and d. purifying and recovering the thus prepared metal dithiene complex.
Claim 2
Dependent Claim
90 words
A process for the synthesis of a transition metal dithiene complex comprising: a. reacting a dimethylaminobenzoin with a phosphorus sulfide and dioxane under suitable reaction conditions to produce a dioxane insoluble thiophosphoric ester derivative of the benzoin; b. adding excess dioxane and dissolving said thiophosphoric ester derivative in a highly polar aprotic solvent; c. reacting said ester derivative dissolved in said aprotic solvent with an aqueous solution of a reactive water soluble ionizable compound of a transition metal complex; and d. purifying and recovering the thus prepared metal dithiene complex.
Claim 3
Dependent Claim
12 words
A process according to claim 1 in which said dimethylaminobenzoin is 4-methoxy-4'-dimethylaminobenzoin.
Claim 4
Dependent Claim
26 words
A process according to claim 1 in which said highly aprotic solvent is selected from the group consisting of N-methyl-pyrrolidinone, diglyme, methyl sulfolane and thiophene dioxide.
Claim 5
Dependent Claim
34 words
A process according to claim 1 wherein said reactive water soluble ionizable compound is selected from the group consisting of NiCl 2 , K 2 PtCl 4 , and K 2 PdCl 4 .
Claim 6
Dependent Claim
17 words
A process according to claim 1 in which said phosphorus sulfide is P 2 S 5 .
Claim 7
Dependent Claim
92 words
A process for the synthesis of a transition metal dithiene complex comprising: a. reacting a dimethylaminobenzoin with a phosphorus sulfide and dioxane under suitable reaction conditions to produce a dioxane insoluble thiophosphoric ester derivative of the benzoin; b. adding excess dioxane and dissolving said thiophosphoric ester derivative in a high boiling point glycol solvent; c. reacting said ester dissolved in said high boiling glycol solvent with an aqueous solution of a reactive water soluble ionizable compound of a transition metal complex; and d. purifying and recovering the thus prepared metal dithiene complex.
Claim 8
Dependent Claim
92 words
A process for the synthesis of a transition metal dithiene complex comprising: a. reacting a dimethylaminobenzoin with a phosphorus sulfide and dioxane under suitable reaction conditions to produce a dioxane insoluble thiophosphoric ester derivative of the benzoin; b. adding excess dioxane and dissolving said thiophosphoric ester derivative in a high boiling point glycol solvent; c. reacting said ester dissolved in said high boiling glycol solvent with an aqueous solution of a reactive water soluble ionizable compound of a transition metal complex; and d. purifying and recovering the thus prepared metal dithiene complex.
Claim 9
Dependent Claim
12 words
A process according to claim 6 in which said dimethylaminobenzoin is 4-methoxy-4'-dimethylaminobenzoin.
Claim 10
Dependent Claim
23 words
A process according to claim 6 in which said high boiling point glycol is an ether alcohol or a monoether of diethylene glycol.
Claim 11
Dependent Claim
34 words
A process according to claim 6 wherein said reactive water soluble ionizable compound is selected from the group consisting of NiCl 2 , K 2 PtCl 4 , and K 2 PdCl 4 .
Claim 12
Dependent Claim
17 words
A process according to claim 6 in which said phosphorus sulfide is P 2 S 5 .
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-06-02 | 1989-12-02 | 1990-06-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-06-02 | 1993-12-02 | 1994-06-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-06-02 | 1997-12-02 | 1998-06-03 | $7700.00 | Window Closed / Lapsed |