IP Library Granted Patent US 7,173,146
Granted Patent B1
US 7,173,146 · App. 11/249,243 · Granted Feb 6, 2007

Menthyl lactate process

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Quick Facts
Patent No.
US 7,173,146
App. No.
11/249,243
Granted
Feb 6, 2007
Kind
B1
Abstract

A simple, high-yield process for making menthyl lactate (ML) is disclosed. Menthol and lactic acid react to produce a mixture comprising menthyl lactate and one or more higher lactoyl esters of ML. Hydrolysis of the esterification mixture follows in the presence of aqueous base under conditions effective to convert the higher lactoyl esters to menthyl lactate. Coincidentally, the conditions minimize hydrolysis of menthyl lactate to menthol, thereby maximizing the overall yield of ML.

Claims (12)

1. A process which comprises:

(a) reacting menthol and lactic acid to produce a mixture comprising menthyl lactate and one or more higher lactoyl esters of menthyl lactate; and

(b) hydrolyzing the mixture in the presence of aqueous base under conditions effective to convert the higher lactoyl esters to menthyl lactate while minimizing hydrolysis of menthyl lactate to menthol.

2. The process of claim 1 wherein the hydrolysis step is performed at a pH less than 14.

3. The process of claim 1 wherein the hydrolysis step is performed at a temperature within the range of about 5° C. to about 70° C.

4. The process of claim 1 wherein the menthyl lactate obtained from hydrolysis is purified by distillation, crystallization, precipitation, sublimation, or a combination thereof.

5. The process of claim 1 wherein the higher lactoyl esters comprise menthyl lactoyl lactate (MLL) and menthyl lactoyl lactoyl lactate (MLLL)

6. A process which comprises hydrolyzing a mixture comprising one or more higher lactoyl esters of menthyl lactate in the presence of aqueous base under conditions effective to convert the higher lactoyl esters to menthyl lactate while minimizing hydrolysis of menthyl lactate to menthol.

7. The process of claim 6 performed at a pH less than 14.

8. The process of claim 6 performed at a temperature from about 5° C. to about 70° C.

9. The process of claim 6 wherein the menthyl lactate obtained from hydrolysis is purified by distillation, crystallization, precipitation, sublimation, or a combination thereof.

10. The process of claim 6 wherein the higher lactoyl esters comprise MLL and MLLL.

Assignments (18)
RELEASE OF SECURITY INTEREST Recorded Feb 1, 2016
From: WELLS FARGO BANK, NATIONAL ASSOCIATION
To: PINOVA HOLDINGS, INC; RENESSENZ LLC
Reel/Frame 037631/0376 →
CHANGE OF NAME Recorded May 9, 2011
From: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
To: RENESSENZ, LLC
Reel/Frame 026246/0863 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 11, 2011
From: MILLENNIUM SPECIALTY CHEMICALS INC.
To: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
Reel/Frame 025619/0024 →
RELEASE OF SECURITY INTEREST Recorded Dec 23, 2010
From: DEUTSCHE BANK TRUST COMPANY AMERICAS, AS COLLATERAL AGENT
To: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
Reel/Frame 025563/0397 →
SECURITY AGREEMENT Recorded Dec 23, 2010
From: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT
Reel/Frame 025562/0245 →
RELEASE OF SECURITY INTEREST Recorded Dec 23, 2010
From: CITIBANK, N.A., AS ADMINISTRATIVE AGENT
To: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
Reel/Frame 025563/0717 →
RELEASE OF SECURITY INTEREST Recorded Dec 23, 2010
From: UBS AG, STAMFORD BRANCH, AS COLLATERAL AGENT
To: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
Reel/Frame 025563/0777 →
RELEASE OF SECURITY INTEREST Recorded Dec 23, 2010
From: WELLS FARGO BANK, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
To: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
Reel/Frame 025563/0798 →
SECURITY AGREEMENT Recorded May 19, 2010
From: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 024402/0727 →
SECURITY AGREEMENT Recorded May 18, 2010
From: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
To: CITIBANK, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 024397/0898 →
SECURITY AGREEMENT Recorded May 7, 2010
From: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
To: UBS AG, STAMFORD BRANCH, AS COLLATERAL AGENT
Reel/Frame 024351/0040 →
SECURITY AGREEMENT Recorded May 6, 2010
From: LYONDELLBASELL FLAVORS & FRAGRANCES, LLC
To: DEUTSCHE BANK TRUST COMPANY AMERICAS, AS COLLATERAL AGENT
Reel/Frame 024342/0135 →
RELEASE OF SECURITY INTEREST Recorded May 5, 2010
From: CITIBANK, N.A., AS COLLATERAL AGENT
To: MILLENNIUM SPECIALTY CHEMICALS INC
Reel/Frame 024337/0090 →
RELEASE OF SECURITY INTEREST Recorded May 5, 2010
From: UBS AG, STAMFORD BRANCH, AS COLLATERAL AGENT
To: MILLENNIUM SPECIALTY CHEMICALS INC.
Reel/Frame 024337/0341 →
SECURITY AGREEMENT Recorded Oct 30, 2009
From: MILLENNIUM SPECIALTY CHEMICALS INC.
To: UBS AG, STAMFORD BRANCH, AS COLLATERAL AGENT
Reel/Frame 023449/0499 →
CORRECTIVE ASSIGNMENT TO CORRECT THE CONVEYING AND RECEIVING PARTIES, PREVIOUSLY RECORDED ON REEL 022520 FRAME 0804. ASSIGNOR(S) HEREBY CONFIRMS THE SECURITY AGREEMENT.. Recorded May 5, 2009
From: MILLENNIUM SPECIALTY CHEMICALS INC.
To: CITIBANK, N.A., AS ADMINISRATIVE AGENT AND COLLATERAL AGENT
Reel/Frame 022634/0303 →
SECURITY AGREEMENT Recorded Apr 9, 2009
From: CITIBANK, N.A., AS ADMINISTRATIVE AGENT AND COLLATERAL AGENT
To: MILLENNIUM SPECIALTY CHEMICALS INC.
Reel/Frame 022520/0804 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 28, 2005
From: ERMAN, MARK B.; SNOW, JOE W.
To: MILLENNIUM SPECIALTY CHEMICALS, INC.
Reel/Frame 017272/0754 →