Patent US4532369A successfully refreshed from Google Patents.
US4532369A
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US
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Process for the preparation of [2,2]-paracyclophane
Assignee: Union Carbide Chemicals and Plastics Technology LLC
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Filing: 1983-10-28
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Granted: 1985-07-30
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Expires: 2003-10-28
Abstract
Abstract A process for the preparation of [2,2]-paracyclophane comprises contacting aqueous p-methylbenzyltrimethylammonium hydroxide with sodium hydroxide or potassium hydroxide, in the presence of dimethyl sulfoxide, and preferably in the further presence of an inert water-immiscible organic solvent.
Inventors
- 👤 Hartmut Hartner
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 21:00
CPC Classifications
C; C07; C07C; C07C1/00; C07C1/32; C07C1/321; C07C1/323; C07C2603/00; C07C2603/92
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
25 words
A process for preparing [2,2]-paracyclophane, comprising the step of contacting aqueous p-methylbenzyltrimethylammonium hydroxide with sodium hydroxide or potassium hydroxide, in the presence of dimethyl sulfoxide.
Claim 2
Dependent Claim
25 words
A process for preparing [2,2]-paracyclophane, comprising the step of contacting aqueous p-methylbenzyltrimethylammonium hydroxide with sodium hydroxide or potassium hydroxide, in the presence of dimethyl sulfoxide.
Claim 3
Dependent Claim
23 words
The process of claim 1, wherein the p-methylbenzyltrimethylammonium hydroxide is generated in situ by contacting aqueous p-methylbenzyltrimethylammonium chloride or bromide with a base.
Claim 4
Dependent Claim
20 words
The process of claim 1, wherein said contacting is effected in the further presence of an inert water-immiscible hydrocarbon solvent.
Claim 5
Dependent Claim
15 words
The process of claim 3, wherein said inert solvent is benzene, toluene, xylene or tetralin.
Claim 6
Dependent Claim
16 words
The process of claim 1, wherein said contacting is effected at a temperature of 50°-130° C.
Claim 7
Dependent Claim
11 words
The process of claim 5, wherein said temperature is 75°-95° C.
Claim 8
Dependent Claim
79 words
The process of claim 1, wherein a concentrated aqueous solution of p-methylbenzyltrimethylammonium chloride is added portionwise, with stirring, to a mixture of 1 volume part 45-50% aqueous sodium hydroxide or potassium hydroxide, 5-50 volume parts toluene and 1-5 volume parts dimethyl sulfoxide, said mixture containing at least a stoichiometric amount of base, at a temperature of 75°-95° C.; stirring and heating at 75°-95° C. is continued for about 10-100 hours; and resultant [2,2]-paracyclophane is recovered from the organic phase.
Claim 9
Dependent Claim
46 words
In a process for preparing [2,2]-paracyclophane by Hofmann elimination, wherein p-methylbenzyltrimethylammonium hydroxide is heated and resultant [2,2]-paracyclophane is recovered, the improvement wherein the reaction is effected by heating aqueous p-methylbenzyltrimethylammonium hydroxide, in contact with an inert water-immiscible organic solvent, and in the presence of dimethyl sulfoxide.
Claim 10
Dependent Claim
46 words
In a process for preparing [2,2]-paracyclophane by Hofmann elimination, wherein p-methylbenzyltrimethylammonium hydroxide is heated and resultant [2,2]-paracyclophane is recovered, the improvement wherein the reaction is effected by heating aqueous p-methylbenzyltrimethylammonium hydroxide, in contact with an inert water-immiscible organic solvent, and in the presence of dimethyl sulfoxide.
Claim 11
Dependent Claim
25 words
The process of claim 8, wherein the p-methylbenzyltrimethylammonium hydroxide is generated in situ by contacting aqueous p-methylbenzyltrimethylammonium chloride or bromide with sodium or potassium hydroxide.
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) | 1988-07-29 | 1989-01-28 | 1989-07-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-07-29 | 1993-01-28 | 1993-07-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-07-29 | 1997-01-28 | 1997-07-30 | $7700.00 | Window Closed / Lapsed |