US5495042A
Expired / Lapsed
US
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Non-alkaline purification of aminophosphonic acids
Assignee: Cytogen Corp
•
Filing: 1993-11-04
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Granted: 1996-02-27
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Expires: 2013-11-04
Abstract
Abstract A process for the purification of aminophosphonic acids under non-alkaline conditions is described. In particular, aminophosphonic acids are slurred in neutral or acidic water, heated to reflux, cooled and then filtered. Product purities approaching 100% are thus obtained.
Inventors
- 👤 Benjamin A. Belinka, Jr.
- 👤 Daniel J. Coughlin
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 18:09
CPC Classifications
C; C07; C07F; C07F9/00; C07F9/02; C07F9/547; C07F9/6524; C07F9/025; C07F9/28; C07F9/38; C07F9/3804; C07F9/3808; C07F9/3817
Claims Analysis
Total Claims: 34
Claim 1
Independent Claim
95 words
A process for the non-alkaline purification of an aminophosphonic acid compound comprising: a) combining a previously prepared aminophosphonic acid compound of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d) filtering said slurry of step c at or below reflux temperature to obtain an aminophosphonic acid compound of greater purity than said previously prepared aminophosphonic acid compound.
Claim 2
Dependent Claim
95 words
A process for the non-alkaline purification of an aminophosphonic acid compound comprising: a) combining a previously prepared aminophosphonic acid compound of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d) filtering said slurry of step c at or below reflux temperature to obtain an aminophosphonic acid compound of greater purity than said previously prepared aminophosphonic acid compound.
Claim 3
Dependent Claim
13 words
The process of claim 1, wherein said aqueous mixture has a neutral pH.
Claim 4
Dependent Claim
13 words
The process of claim 1, wherein said aqueous mixture has an acidic pH.
Claim 5
Dependent Claim
24 words
The process of claim 1, wherein said aminophosphonic acid compound is selected from the group consisting of EDTMP, DOTMP, DTPMP, NTMP, HEEDTMP, and TTHMP.
Claim 6
Dependent Claim
12 words
The process of claim 1, wherein the aminophosphonic acid compound is DTPMP.
Claim 7
Dependent Claim
12 words
The process of claim 1, wherein the aminophosphonic acid compound is NTMP.
Claim 8
Dependent Claim
12 words
The process of claim 1, wherein the aminophosphonic acid compound is HEEDTMP.
Claim 9
Dependent Claim
12 words
The process of claim 1, wherein the aminophosphonic acid compound is TTHMP.
Claim 10
Dependent Claim
27 words
The process of claim 1, in which said aqueous mixture of step (c) is allowed to cool to a temperature below reflux prior to performing step (d).
Claim 11
Dependent Claim
18 words
The process of claim 9, wherein the temperature below reflux ranges from about 70° to about 90° C.
Claim 12
Dependent Claim
14 words
The process of claim 10, wherein the temperature below reflux is about 80° C.
Claim 13
Dependent Claim
26 words
The process of claim 1, wherein the filtration of said aqueous mixture is carried out at a temperature ranging from about 70° to about 90° C.
Claim 14
Dependent Claim
22 words
The process of claim 12, wherein the filtration of said aqueous mixture is carried out at a temperature of about 80° C.
Claim 15
Dependent Claim
85 words
A process for the non-alkaline purification of EDTMP comprising: a) combining a previously prepared EDTMP of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d) filtering said slurry of step c at or below reflux temperature to obtain EDTMP of greater purity than said previously prepared EDTMP.
Claim 16
Dependent Claim
85 words
A process for the non-alkaline purification of EDTMP comprising: a) combining a previously prepared EDTMP of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d) filtering said slurry of step c at or below reflux temperature to obtain EDTMP of greater purity than said previously prepared EDTMP.
Claim 17
Dependent Claim
85 words
A process for the non-alkaline purification of DOTMP comprising: a) combining a previously prepared DOTMP of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d) filtering said slurry of step c at or below reflux temperature to obtain DOTMP of greater purity than said previously prepared DOTMP.
Claim 18
Dependent Claim
85 words
A process for the non-alkaline purification of DOTMP comprising: a) combining a previously prepared DOTMP of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d) filtering said slurry of step c at or below reflux temperature to obtain DOTMP of greater purity than said previously prepared DOTMP.
Claim 19
Dependent Claim
16 words
The process of claim 1, in which step (c) is maintained for up to 72 hours.
Claim 20
Dependent Claim
16 words
The process of claim 1, in which step (c) is maintained for up to 48 hours.
Claim 21
Dependent Claim
16 words
The process of claim 1, in which step (c) is maintained for up to 24 hours.
Claim 22
Dependent Claim
16 words
The process of claim 14, in which step (c) is maintained for up to 48 hours.
Claim 23
Dependent Claim
16 words
The process of claim 15, in which step (c) is maintained for up to 48 hours.
Claim 24
Dependent Claim
91 words
A process for the non-alkaline purification of an aminophosphonic acid compound comprising: a) combining a previously prepared aminophosphonic acid compound of a given purity and water having an acidic, not alkaline, pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d)filtering said slurry of step c at or below reflux temperature to obtain an aminophosphonic acid compound of greater purity than said previously prepared aminophosphonic acid compound.
Claim 25
Dependent Claim
91 words
A process for the non-alkaline purification of an aminophosphonic acid compound comprising: a) combining a previously prepared aminophosphonic acid compound of a given purity and water having an acidic, not alkaline, pH to form a slurry; b) heating said slurry to reflux; c) maintaining said slurry at reflux for a period of time in the range of about 1 to about 96 hours; and d)filtering said slurry of step c at or below reflux temperature to obtain an aminophosphonic acid compound of greater purity than said previously prepared aminophosphonic acid compound.
Claim 26
Dependent Claim
74 words
A process for the non-alkaline purification of an aminophosphonic acid compound comprising: a) combining a previously prepared aminophosphonic acid compound of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; and c) filtering said slurry of step (b) at or below reflux temperature to obtain an aminophosphonic acid compound of greater purity than said previously prepared aminophosphonic acid compound.
Claim 27
Dependent Claim
74 words
A process for the non-alkaline purification of an aminophosphonic acid compound comprising: a) combining a previously prepared aminophosphonic acid compound of a given purity and water having a neutral or acidic but not alkaline pH to form a slurry; b) heating said slurry to reflux; and c) filtering said slurry of step (b) at or below reflux temperature to obtain an aminophosphonic acid compound of greater purity than said previously prepared aminophosphonic acid compound.
Claim 28
Dependent Claim
23 words
The process of claim 22 which further comprises stirring said slurry at reflux for a period of time prior to said filtering step.
Claim 29
Dependent Claim
17 words
The process of claim 23 in which said slurry is stirred at reflux for about 1 hour.
Claim 30
Dependent Claim
17 words
The process of claim 23 in which said slurry is stirred at reflux for about 24 hours.
Claim 31
Dependent Claim
25 words
The process of claim 22 in which said aminophosphonic acid compound is selected from the group consisting of EDTMP, DOTMP, DTPMP, NTMP, HEEDTMP or TTHMP.
Claim 32
Dependent Claim
13 words
The process of claim 22 in which said aminophosphonic acid compound is EDTMP.
Claim 33
Dependent Claim
13 words
The process of claim 23 in which said aminophosphonic acid compound is EDTMP.
Claim 34
Dependent Claim
13 words
The process of claim 22 in which said water has an acidic pH.
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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) | 1999-02-26 | 1999-08-28 | 2000-02-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2003-02-26 | 2003-08-28 | 2004-02-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2007-02-26 | 2007-08-28 | 2008-02-27 | $7700.00 | Window Closed / Lapsed |