US4474975A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for producing tris (N-methylamino) methylsilane
Assignee: United States, NASA THE, Administrator of
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Filing: 1983-05-09
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Granted: 1984-10-02
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Expires: 2003-05-09
Abstract
Abstract A method of producing tris (N-methylamine) methylsilane, including the steps of forming and cooling a liquid solution of methylamine in an inert solvent and under an inert atmosphere at a temperature of about -30° C. and slowly adding a quantity of methyltrichlorosilane while maintaining said temperature. The reaction mixture is then heated for about 60 minutes at a temperature of about 40° C., followed by filtering the solid portion from the liquid portion. The liquid is distilled to remove the solvent, resulting in a high yield of tris (N-methylamine) methylsilane.
Inventors
- 👤 Johnny M. Clemons
- 👤 Benjamin G. Penn
- 👤 Frank E. Ledbetter, III
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 16:46
CPC Classifications
C; C07; C07F; C07F7/00; C07F7/02; C07F7/08; C07F7/10; C08; C08G; C08G77/00; C08G77/60; C08G77/62
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
94 words
In the method of producing tris (N-methylamino) methyl silane which comprises reacting methyltrichlorosilane with methylamine in an organic solvent by heating a reaction mixture thereof and purifying the resulting product by distillation, the improvement comprising: (a) forming said reaction mixture by preparing a liquid solution of methyl amine in said solvent at a temperature of less than -20° C. and slowly admixing in said solution a quantity of methyltrichorosilane while maintaining said temperature and (b) filtering the reaction mixture after reacting the same and prior to distillation so as to remove insoluble by-product material.
Claim 2
Dependent Claim
94 words
In the method of producing tris (N-methylamino) methyl silane which comprises reacting methyltrichlorosilane with methylamine in an organic solvent by heating a reaction mixture thereof and purifying the resulting product by distillation, the improvement comprising: (a) forming said reaction mixture by preparing a liquid solution of methyl amine in said solvent at a temperature of less than -20° C. and slowly admixing in said solution a quantity of methyltrichorosilane while maintaining said temperature and (b) filtering the reaction mixture after reacting the same and prior to distillation so as to remove insoluble by-product material.
Claim 3
Dependent Claim
16 words
The improvement of claim 1 wherein said method is carried out under a dry inert atmosphere.
Claim 4
Dependent Claim
18 words
The method of claim 2 wherein said inert atmosphere is nitrogen and said inert solvent is petroleum ether.
Claim 5
Dependent Claim
22 words
The method of claim 1 where said solution is maintained at a temperature of from about -20° C. to about -50° C.
Claim 6
Dependent Claim
12 words
The method of claim 4 wherein said temperature is about -30° C.
Claim 7
Independent Claim
114 words
A method of producing tris (N-methylamino) methylsilane, comprising the steps of: (a) forming and cooling a liquid solution of methylamine in an inert atmosphere and in an inert solvent at a temperature of about -30° C.; (b) slowly admixing a quantity of methyltrichlorosilane to said solution while maintaining said temperature to form a reaction mixture in said inert atmosphere; (c) heating said reaction mixture at a temperature of about 40° C. for about 60 minutes to produce a solid portion and a liquid portion; (d) filtering said liquid portion from said solid portion while maintaining said inert atmosphere; and (e) distilling the liquid portion under pressure in said inert atmosphere to remove said solvent.
Claim 8
Independent Claim
114 words
A method of producing tris (N-methylamino) methylsilane, comprising the steps of: (a) forming and cooling a liquid solution of methylamine in an inert atmosphere and in an inert solvent at a temperature of about -30° C.; (b) slowly admixing a quantity of methyltrichlorosilane to said solution while maintaining said temperature to form a reaction mixture in said inert atmosphere; (c) heating said reaction mixture at a temperature of about 40° C. for about 60 minutes to produce a solid portion and a liquid portion; (d) filtering said liquid portion from said solid portion while maintaining said inert atmosphere; and (e) distilling the liquid portion under pressure in said inert atmosphere to remove said solvent.
Claim 9
Dependent Claim
18 words
The method of claim 6 wherein said inert atmosphere is nitrogen and said inert solvent is petroleum ether.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1987-10-02 | 1988-04-02 | 1988-10-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-10-02 | 1992-04-02 | 1992-10-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-10-02 | 1996-04-02 | 1996-10-02 | $7700.00 | Window Closed / Lapsed |