IP Library Granted Patent US 6,906,220
Granted Patent B2
US 6,906,220 · App. 10/396,085 · Granted Jun 14, 2005

Process to produce 4-(2-sulfoethyl) cyclohexane, 1,2-diol sodium salt from 4-vinylcyclohexane-1,2-diol

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Quick Facts
Patent No.
US 6,906,220
App. No.
10/396,085
Granted
Jun 14, 2005
Kind
B2
Abstract

Disclosed herein is a process for preparing 4-(2-sulfoethylcyclohexane)-1,2-diol sodium salt, at ambient condition and in the presence of a buffer and an initiator, from vinylcyclohexane-1,2-diol. Also disclosed is a process for preparing 3-(2-sulfoethyl) hexanedioic acid, sodium salt by oxidizing 4-(2-sulfoethylcyclohexane)-1,2 diol sodium salt with hydrogen peroxide in the presence of tungstic acid.

Claims (14)

1. A process for making 4-(2-sulfoethyl) cyclohexane-1,2 diol sodium salt, said process comprising:

contacting 4-vinylcyclohexane-1,2-diol with a sulfonating agent in the presence of a buffer solution and an initiator, at ambient conditions, wherein the sulfonating agent is selected from the group consisting of sodium bisulfate and ammonium bisulfate and wherein the buffer solution is selected from the group consisting of alkali metal and ammonium phosphate, bicarbonates, and acetates.

2. The process of claim 1 wherein the sulfonating agent comprises sodium bisulfate.

3. The process of claim 1 , wherein the buffer solution is selected from the group consisting of potassium phosphate, potassium acetate, ammonium phosphate, ammonium bicarbonate, ammonium acetate, sodium phosphate, sodium bicarbonate and sodium acetate.

4. The process of claim 1 , wherein the initiator is selected from the group consisting of hydrogen peroxide, sodium persulfate and potassium persulfate.

5. The process of claim 1 , wherein the 4-vinylcyclohexane-1,2-diol is prepared by a process comprising:

contacting 4-vinylcyclohexane-1,2-epoxide with water in the presence of a solid acidic catalyst at ambient conditions for a time sufficient to produce 4-vinylcyclohexane-1,2-diol.

6. The process of claim 1 , wherein 4-vinylcyclohexane-1,2-diol is prepared by a process comprising:

contacting 4-vinylcyclohexane with formic acid in the presence of hydrogen peroxide to form a mixture A comprising at least one of 4-vinylcyclohexane 1,2-diformate, 4-vinylcyclohexane 1-formate 2-ol, 4-vinylcyclohexane 1-ol 2-formate, and 4-vinylcyclohexane-1,2-diol;

contacting mixture A with sodium hydroxide to accomplish hydrolysis of at least a portion of the compounds in mixture A to produce a mixture B comprising an aqueous phase and an organic phase; and

separating the aqueous phase from the organic phase in mixture B, and obtaining an organic phase comprising essentially of 4-vinylcyclohexane 1,2-diol.

7. A process for making 3-(2-sulfoethyl) hexanedioic acid, sodium salt comprising: oxidizing 4-(2-sulfoethylcyclohexane)-1,2 diol sodium salt made by the process of claim 1 with hydrogen peroxide in the presence of tungstic acid.

8. The process of claim 1 , wherein the buffer solution comprises ammonium phosphate.

9. The process of claim 1 , wherein the buffer solution comprises sodium phosphate.

Assignments (6)
RELEASE OF SECURITY INTEREST Recorded Nov 10, 2011
From: DEUTSCHE BANK AG NEW YORK BRANCH
To: INVISTA NORTH AMERICA S.A.R.L.
Reel/Frame 027211/0298 →
SECURITY AGREEMENT Recorded Mar 19, 2009
From: INVISTA NORTH AMERICA S.A.R.L.
To: DEUTSCHE BANK AG NEW YORK BRANCH, AS COLLATERAL AGENT
Reel/Frame 022416/0849 →
RELEASE OF U.S. PATENT SECURITY INTEREST Recorded Mar 19, 2009
From: JPMORGAN CHASE BANK, N.A., AS ADMINISTRATIVE AGENT AND COLLATERAL AGENT (F/K/A JPMORGAN CHASE BANK)
To: INVISTA NORTH AMERICA S.A.R.L. (F/K/A ARTEVA NORTH AMERICA S.A.R.L.)
Reel/Frame 022427/0001 →
SECURITY INTEREST Recorded Jun 23, 2004
From: INVISTA NORTH AMERICA S.A.R.L. F/K/A ARTEVA NORTH AMERICA S.A.R.
To: JPMORGAN CHASE BANK, N.A.
Reel/Frame 015592/0824 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 27, 2004
From: E. I. DU PONT DE NEMOURS AND COMPANY
To: INVISTA NORTH AMERICA S.A.R.L.
Reel/Frame 015286/0708 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 27, 2003
From: SUN, YANHUI; CHEN, SHAORONG
To: E. I. DU PONT DE NEMOURS AND COMPANY
Reel/Frame 013764/0660 →