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US4590014A
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Synthesis of alkyl phosphinate salts
Assignee: Ecolab Inc
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Filing: 1984-09-06
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Granted: 1986-05-20
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Expires: 2004-09-06
Abstract
Abstract An improved method for the preparation of alkali metal phosphinate salts by the reaction of an olefinic material with an alkali metal hypophosphite in the presence of a free radical source is disclosed.
Inventors
- 👤 Stephen F. Wolf
- 👤 Chung-Tsing Liu
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 09:55
CPC Classifications
C; C07; C07F; C07F9/00; C07F9/02; C07F9/28; C07F9/30; C07F9/48
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
106 words
A method for the preparation of alkyl phosphinate salts by the reaction of an olefinic material with an alkali metal hypophosphite in the presence of an organic peroxyester free radical source comprising: (a) simultaneously adding an alcoholic solution of the olefinic material and an alcoholic solution containing essentially all of the free radical source or a mixture thereof to a reaction medium comprising an aqueous alcoholic solution of the hypophosphite, while maintaining the hypophosphite solution at about 50°-100° C. during the addition; and (b) heating the combined solutions at 50°-100° C. for about 1.5-6.0 hours to afford about an 80-100% yield of the alkyl phosphinate salt.
Claim 2
Independent Claim
106 words
A method for the preparation of alkyl phosphinate salts by the reaction of an olefinic material with an alkali metal hypophosphite in the presence of an organic peroxyester free radical source comprising: (a) simultaneously adding an alcoholic solution of the olefinic material and an alcoholic solution containing essentially all of the free radical source or a mixture thereof to a reaction medium comprising an aqueous alcoholic solution of the hypophosphite, while maintaining the hypophosphite solution at about 50°-100° C. during the addition; and (b) heating the combined solutions at 50°-100° C. for about 1.5-6.0 hours to afford about an 80-100% yield of the alkyl phosphinate salt.
Claim 3
Dependent Claim
26 words
The method of claim 1 wherein the free radical source is an alkyl ester of a peroxycarboxylic acid or an alkyl ester of a monoperoxydicarboxylic acid.
Claim 4
Dependent Claim
14 words
The method of claim 1 wherein the reaction medium and the solution comprise ethanol.
Claim 5
Dependent Claim
18 words
The method of claim 3 wherein the reaction medium comprises about a 3:1 mixture of ethanol and water.
Claim 6
Dependent Claim
18 words
The method of claim 1 wherein the olefin is an alpha-olefin and the hypophosphite is sodium hypophosphite monohydrate.
Claim 7
Dependent Claim
15 words
The method of claim 1 wherein the olefin is an olefinic dicarboxylic acid or ester.
Claim 8
Dependent Claim
19 words
The method of claim 1 wherein the ratio of ethanol to water in the combined solutions is about 2-8:1.
Claim 9
Dependent Claim
17 words
The method of claim 1 wherein the combined solutions are heated at 50°-100° C. for 3-6 hours.
Claim 10
Dependent Claim
23 words
The method of claim 1 wherein the olefinic material is a C 6 -C 22 -alpha-olefin or a C 5 -C 8 -cycloalkene.
Claim 11
Dependent Claim
17 words
The method of claim 1 wherein the mole ratio of olefinic material to hypophosphite is about 1:1.
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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) | 1989-05-19 | 1989-11-18 | 1990-05-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-05-19 | 1993-11-18 | 1994-05-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-05-19 | 1997-11-18 | 1998-05-20 | $7700.00 | Window Closed / Lapsed |