← Back to Patent Explorer
US5488154A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the preparation of alkoxyalkanoic acids

Assignee: Shell USA Inc
•
Filing: 1994-10-13
•
Granted: 1996-01-30
•
Expires: 2014-10-13
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract A process for the preparation of an alkoxyalkanoic acid by reacting the corresponding alkoxyalkanol with a stable free radical nitroxide in the presence of a chromium (II) salt, a highly polar solvent, an oxidant and water, at a temperature in the range of from about 0° C. to about 100° C. and thereafter separating out the alkoxyalkanoic acid.

Inventors

  • 👤 Herbert E. Fried

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 20:55
CPC Classifications
C; C07; C07C; C07C51/00; C07C51/16; C07C51/27

Claims Analysis

Total Claims: 20
Claim 1
Independent Claim 303 words
A process for the preparation of an alkoxyalkanoic acid of the formula RO(CH 2 CHR'O) n CH 2 CO 2 H wherein R is an alkyl group of from about 1 to about 1000 carbon atoms, R' is hydrogen or alkyl or mixtures thereof (on the individual molecule) and n is an integer of from about 1 to about 1000, which comprises reacting the corresponding alkoxyalkanol with a stable free radical nitroxide having the formula: ##STR16## wherein (1) (a) each of R 1 , R 2 , R 3 and R 4 is an alkyl, aryl or substituted alkyl group having 1 to about 15 carbon atoms, and (b) R 5 and R 6 (i) each is an alkyl group having 1 to about 15 carbon atoms provided that R 1 -R 6 are not all alkyl groups, or a substituted alkyl group having 1 to about 15 carbon atoms wherein the substituent is hydrogen, cyano, --CONH 2 , --OCOCH 3 , OCOC 2 H 5 , carbonyl, alkenyl wherein the double bond is not conjugated with the nitroxide moiety, or --COOR wherein R of the --COOR group is alkyl or aryl, or (ii) together form part of a ring that contains at least 3 carbon atoms and up to two heteroatoms of O or N, (2) the ##STR17## moiety and the ##STR18## moiety individually are aryl, or (3) the ##STR19## moiety and the ##STR20## moiety together form a bicyclic ring with the proviso that the group directly adjacent to the N--O moiety is a bridgehead C--H, or a fully alkylated carbon, in the presence of a chromium (II) salt, a nitrite compound, a highly polar solvent, an oxidant and water, at a temperature in the range of from about 0° C. to about 100° C. and thereafter separating out the alkoxyalkanoic acid.
Claim 2
Dependent Claim 303 words
A process for the preparation of an alkoxyalkanoic acid of the formula RO(CH 2 CHR'O) n CH 2 CO 2 H wherein R is an alkyl group of from about 1 to about 1000 carbon atoms, R' is hydrogen or alkyl or mixtures thereof (on the individual molecule) and n is an integer of from about 1 to about 1000, which comprises reacting the corresponding alkoxyalkanol with a stable free radical nitroxide having the formula: ##STR16## wherein (1) (a) each of R 1 , R 2 , R 3 and R 4 is an alkyl, aryl or substituted alkyl group having 1 to about 15 carbon atoms, and (b) R 5 and R 6 (i) each is an alkyl group having 1 to about 15 carbon atoms provided that R 1 -R 6 are not all alkyl groups, or a substituted alkyl group having 1 to about 15 carbon atoms wherein the substituent is hydrogen, cyano, --CONH 2 , --OCOCH 3 , OCOC 2 H 5 , carbonyl, alkenyl wherein the double bond is not conjugated with the nitroxide moiety, or --COOR wherein R of the --COOR group is alkyl or aryl, or (ii) together form part of a ring that contains at least 3 carbon atoms and up to two heteroatoms of O or N, (2) the ##STR17## moiety and the ##STR18## moiety individually are aryl, or (3) the ##STR19## moiety and the ##STR20## moiety together form a bicyclic ring with the proviso that the group directly adjacent to the N--O moiety is a bridgehead C--H, or a fully alkylated carbon, in the presence of a chromium (II) salt, a nitrite compound, a highly polar solvent, an oxidant and water, at a temperature in the range of from about 0° C. to about 100° C. and thereafter separating out the alkoxyalkanoic acid.
Claim 3
Dependent Claim 21 words
The process of claim 1 wherein said alkoxyalkanol has a carbon number in the range from about 11 to about 18.
Claim 4
Dependent Claim 24 words
The process of claim 1 wherein the stable free radical nitroxide is selected from the group consisting of 2,2,6,6,-tetramethylpiperidine-1-oxyl, 2,2,5,5-tetramethylpyrrolidin-1-oxyl, 2,2,7,7-tetramethylcycloheptan-1-oxyl, and mixtures thereof.
Claim 5
Dependent Claim 61 words
The process of claim 1 wherein the stable free radical nitroxide has the formula: ##STR21## wherein each of R 7 , R 8 , R 9 and R 10 is an alkyl, aryl or substituted alkyl group having 1 to about 15 carbon atoms and each of R 11 , and R 12 is alkyl, hydrogen, aryl or a substituted heteroatom.
Claim 6
Dependent Claim 31 words
The process of claim 4 wherein the stable free radical nitroxide is selected from the group consisting of 2,2,6,6-tetramethylpiperidine-1-oxyl, 4-methoxy-2,2,6,6-tetramethylpiperidine-1-oxyl, 4-ethoxy-2,2,6,6-tetramethylpiperidine-1-oxyl, 4-acetylamino-2,2,6,6-tetramethylpiperidine-1-oxyl, 4-carbamoyl-2,2,6,6-tetramethylpiperidine-1-oxyl, 4-benzoylamino-2,2,6,6-tetra-methylpiperidine-1-oxyl, 4-pivaloylamido-2,2,6,6-tetramethylpiperidine-1-oxyl, 4-dodecyloylamido-2,2,6,6-tetramethylpiperidine-1-oxyl, 4-dodecanoylamino-2,2,6,6tetramethylpiperidine-1-oxyl, 4-octanoylamino-2,2,6,6-tetramethylpiperidine-1-oxyl and mixtures thereof.
Claim 7
Dependent Claim 25 words
The process of claim 5 wherein the stable free radical nitroxide is selected from the group consisting of 2,2,6,6-tetramethylpiperidine-1-oxyl, 4-acetylamino-2,2,6,6-tetramethylpiperidine-1-oxyl, 4-methoxy-2, 2,6,6-tetramethylpiperidine-1-oxyl and mixtures thereof.
Claim 8
Dependent Claim 32 words
The process of claim 1 wherein said chromium (II) salt is selected from the group consisting of chromium (II) chloride, chromium (II) bromide, chromium (II) iodide, chromium (II) sulfate, and mixtures thereof.
Claim 9
Dependent Claim 22 words
The process of claim 1 wherein the solvent is selected from the group of acetonitrile, sulfolane, N-methylpyrrolidinone, acetic acid and mixtures thereof.
Claim 10
Dependent Claim 10 words
The process of claim 8 wherein the solvent is acetonitrile.
Claim 11
Dependent Claim 23 words
The process of claim 1 wherein said nitrite compound is selected from the group consisting of sodium nitrite, potassium nitrite and mixtures thereof.
Claim 12
Dependent Claim 12 words
The process of claim 10 wherein said nitrite compound is sodium nitrite.
Claim 13
Dependent Claim 32 words
The process of claim 1 wherein the amount of nitrite compound is in the range of from about 5 mole percent to about 500 mole percent, basis the moles of starting alkoxyalkanol.
Claim 14
Dependent Claim 33 words
The process of claim 1 wherein said alkoxyalkanol is contacted with said stable free radical nitroxide and said solvent, followed by the addition thereto of said nitrite compound and said chromium (II) salt.
Claim 15
Dependent Claim 35 words
The process of claim 13 wherein the amount of stable free radical nitroxide is in the range of from about 0.01 mole percent to about 200 mole percent, basis the number of moles of alkoxyalkanol.
Claim 16
Dependent Claim 33 words
The process of claim 13 wherein the amount of nitrite compound is in the range of from about 5 mole percent to about 20 mole percent, basis the number of moles of alkoxyalkanol.
Claim 17
Dependent Claim 12 words
The process of claim 1 wherein said oxidant is an oxygen-containing gas.
Claim 18
Dependent Claim 20 words
The process of claim 16 wherein said oxygen-containing gas is selected from the group consisting of pure oxygen and air.
Claim 19
Dependent Claim 31 words
The process of claim 1 wherein the amount of water is in the range of from about 10 mole percent to about 1000 mole percent, basis the moles of starting alkoxyalkanol.
Claim 20
Dependent Claim 30 words
The process of claim 1 wherein said process is carried out at a temperature in the range of from about 20° C. to about 70° C. and at atmospheric pressure.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1999-01-29 1999-07-31 2000-01-30 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2003-01-29 2003-07-31 2004-01-30 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2007-01-29 2007-07-31 2008-01-30 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag