IP Library Granted Patent US 8,841,408
Granted Patent B2
US 8,841,408 · App. 12/106,429 · Granted Sep 23, 2014

Macromonomers and hydrogel systems using native chemical ligation, and their methods of preparation

Inventors: Phillip B Messersmith (Clarendon Hills, IL); Bi-Huang Hu (Chicago, IL); Jing Su (Chicago, IL)
Assignee: Northwestern University
C08G69/40C08G69/02C08G69/04C08G69/08
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Quick Facts
Patent No.
US 8,841,408
App. No.
12/106,429
Granted
Sep 23, 2014
Kind
B2
Abstract

Biocompatible macromonomers, hydrogels, methods of synthesis and methods of use thereof are provided. The biocompatible hydrogels of the present invention are prepared using native chemical ligation (NCL), in which a thioester readily reacts with a N-terminal thiol (cysteine) through transesterification and rearrangement to form an amide bond through a five-member ring intermediate.

Claims (37)

1. A macromonomer comprising the structure:

wherein each “n” has a value in the range of from 0 to 200.

2. A method of synthesizing a hydrogel comprising the structure:

wherein each “n” has a value in the range of from 0 to 200, the method comprising covalently crosslinking through native chemical ligation an effective amount of the macromonomer of claim 1 with an effective amount of a second macromonomer having the structure:

wherein each “n” has a value in the range of 0 to 200;

whereby the hydrogel and a thiol byproduct are formed.

3. The method of claim 2 wherein equivalent amounts of the macromonomer of claim 1 and of the second macromonomer are used.

4. A method of synthesizing a biocompatible hydrogel comprising the structure:

wherein each “n” has a value in the range of from 0 to 200, the method comprising covalently crosslinking through native chemical ligation an effective amount of the macromonomer of claim 1 with an effective amount of a second macromonomer having the structure:

wherein each “n” has a value in the range of 0 to 200 and wherein R is hydrogen;

whereby the biocompatible hydrogel and a thiol byproduct are formed.

5. A method of synthesizing a biocompatible hydrogel comprising the structure:

wherein each “n” has a value in the range of from 0 to 200, the method comprising covalently crosslinking through native chemical ligation an effective amount of the macromonomer of claim 1 with an effective amount of a second macromonomer having the structure:

wherein each “n” has a value in the range of 0 to 200 and wherein R is CH 2 CH 7 COOH;

whereby the biocompatible hydrogel and a thiol byproduct are formed.

6. A method of synthesizing a biocompatible hydrogel comprising the structure:

wherein each “n” has a value in the range of from 0 to 200, the method comprising covalently crosslinking through native chemical ligation an effective amount of the macromonomer of claim 1 with an effective amount of a second macromonomer having the structure:

wherein each “n” has a value in the range of 0 to 200 and wherein R is CH 2 COOH;

whereby the biocompatible hydrogel and a thiol byproduct are formed.

7. A method of synthesizing a biocompatible hydrogel comprising the structure:

wherein each “n” has a value in the range of from 0 to 200, the method comprising covalently crosslinking through native chemical ligation an effective amount of the macromonomer of claim 1 with an effective amount of a second macromonomer having the structure:

wherein each “n” has a value in the range of 0 to 200 and wherein R is

whereby the biocompatible hydrogel and a thiol byproduct are formed.

8. A method of synthesizing a biocompatible hydrogel comprising the structure:

wherein each “n” has a value in the range of from 0 to 200, the method comprising covalently crosslinking through native chemical ligation an effective amount of the macromonomer of claim 1 with an effective amount of a second macromonomer having the structure:

wherein each “n” has a value in the range of 0 to 200 and wherein R is (CH 2 ) 3 NH(NH)CNH 2 ;

whereby the biocompatible hydrogel and a thiol byproduct are formed.

9. A method of synthesizing a macromonomer comprising the structure:

wherein each “n” has a value in the range of from 0 to 200, the method comprising:

(a) preparing a thioester, wherein the thioester is Ethyl 3-Mercaptoproprionate-Succinnic Acid (EMPSA); and

(b) coupling the thioester with an amine-terminated 4-armed poly(ethylene glycol); wherein the macromonomer is formed.

10. A hydrogel produced by native chemical ligation of the macromonomer of claim 1 to a macromonomer having the formula:

wherein each “n” has a value in the range of 0 to 200;

wherein the hydrogel comprises the following structure:

11. A hydrogel produced by native chemical ligation of the macromonomer of claim 1 to a macromonomer having the formula:

wherein each “n” has a value in the range of 0 to 200 and wherein “R” is selected from the group consisting of H, CH 2 CH 2 COOH, CH 2 COOH, (CH 2 ) 3 NH(NH)CNH 2 and

wherein the hydrogel comprises the following structure:

Assignments (4)
CONFIRMATORY LICENSE Recorded May 11, 2023
From: NORTHWESTERN UNIVERSITY
To: NIH - DEITR
Reel/Frame 063617/0621 →
CONFIRMATORY LICENSE Recorded Jan 21, 2015
From: NORTHWESTERN UNIVERSITY
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 034767/0309 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 5, 2008
From: MESSERSMITH, PHILLIP B.; HU, BI-HUANG; SU, JING
To: NORTHWESTERN UNIVERSITY
Reel/Frame 020899/0641 →
CONFIRMATORY LICENSE Recorded Apr 23, 2008
From: NORTHWESTERN UNIVERSITY
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 020842/0475 →
Continuity (2)
Provisional Application 60925496 · Apr 19, 2007
Related Publication 20080274980A1 · Nov 6, 2008