Patent US4258197A successfully refreshed from Google Patents.
US4258197A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Manufacture of sulfenamides
Assignee: Pennwalt Corp
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Filing: 1979-06-08
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Granted: 1981-03-24
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Expires: 1999-06-08
Abstract
Abstract Processes for the manufacture of sulfenamides by the oxidation of a mixture of 2-mercaptobenzothiazole and the appropriate amine in a critical amount of water and/or organic solvent produces a pure product of good quality and high yield. The amount of water should be in the range of from 10 to 30% by weight based on the total reaction mixture.
Inventors
- 👤 Sameeh S. Toukan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 09:39
CPC Classifications
C; C07; C07D; C07D277/00; C07D277/60; C07D277/62; C07D277/68; C07D277/70; C07D277/76; C07D277/80
Claims Analysis
Total Claims: 6
Claim 1
Independent Claim
162 words
A process for the manufacture of 2-benzothiazole-sulfenamides consisting essentially of: adding 10 to 30 percent by weight of a member selected from the group consisting of water, 20 to 60 percent by weight of ethylene glycol monoalkyl ether solvent, and a mixture thereof to one mole of 2-mercaptobenzathiazole and cooling the mixture to 8°-12° C.; adding dropwise 1.5 to 4 moles of a primary or secondary amine selected from the group consisting of morpholine, tert-butylamine, isopropylamine, diisopropylamine and cyclohexylamine to the mercaptobenzothiazole-water mixture while maintaining a temperature below 20° C.; adding 1.5 to 2 moles of an oxidizing agent selected from the group consisting of chlorine, alkali metal hypochlorites, and hydrogen peroxide slowly to the mercaptobenzothiazoleamine-water mixture while maintaining the temperature of the solution in the range of 25° to 60° C. until the oxidation is completed; cooling the oxidized reaction mixture to about 5° to 15° C. whereby the sulfenamide product precipitates; and recovering the sulfenamide product in substantially pure form.
Claim 2
Dependent Claim
162 words
A process for the manufacture of 2-benzothiazole-sulfenamides consisting essentially of: adding 10 to 30 percent by weight of a member selected from the group consisting of water, 20 to 60 percent by weight of ethylene glycol monoalkyl ether solvent, and a mixture thereof to one mole of 2-mercaptobenzathiazole and cooling the mixture to 8°-12° C.; adding dropwise 1.5 to 4 moles of a primary or secondary amine selected from the group consisting of morpholine, tert-butylamine, isopropylamine, diisopropylamine and cyclohexylamine to the mercaptobenzothiazole-water mixture while maintaining a temperature below 20° C.; adding 1.5 to 2 moles of an oxidizing agent selected from the group consisting of chlorine, alkali metal hypochlorites, and hydrogen peroxide slowly to the mercaptobenzothiazoleamine-water mixture while maintaining the temperature of the solution in the range of 25° to 60° C. until the oxidation is completed; cooling the oxidized reaction mixture to about 5° to 15° C. whereby the sulfenamide product precipitates; and recovering the sulfenamide product in substantially pure form.
Claim 3
Dependent Claim
27 words
A process according to claim 1 in which the oxidizing agent is an alkali metal hypochlorite and which is carried out in a range of 20°-60° C.
Claim 4
Dependent Claim
17 words
A process according to claim 1 where the oxidation is carried out in an entirely aqueous medium.
Claim 5
Dependent Claim
15 words
A process according to claim 3 where the organic solvent is ethylene glycol monobutyl ether.
Claim 6
Dependent Claim
23 words
A process according to claim 1 where the oxidation is carried out in a mixture of water and ethylene glycol monoalkyl ether solvent.
References Cited (Backward Citations)
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US2271834A
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GB655668A
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US2354427A
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US2419283A
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GB772582A
Cited
US3600398A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-03-23 | 1984-09-22 | 1985-03-24 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-03-23 | 1988-09-22 | 1989-03-24 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-03-23 | 1992-09-22 | 1993-03-24 | $7700.00 | Window Closed / Lapsed |