IP Library Granted Patent US 8,877,939
Granted Patent B2
US 8,877,939 · App. 14/078,106 · Granted Nov 4, 2014

Copper-catalysed ligation of azides and acetylenes

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Quick Facts
Patent No.
US 8,877,939
App. No.
14/078,106
Granted
Nov 4, 2014
Kind
B2
Abstract

A copper catalyzed click chemistry ligation process is employed to bind azides and terminal acetylenes to provide 1,4-disubstituted 1,2,3-triazole triazoles. The process comprises contacting an organic azide and a terminal alkyne with a source of reactive Cu(I) ion in human blood plasma to form by cycloaddition a 1,4-disubstituted 1,2,3-triazole. The source of reactive Cu(I) ion can be, for example, a Cu(I) salt, Cu(II) ion in the presence of a reducing agent, or copper metal.

Claims (23)

1. A copper catalyzed process for preparing a 1,4-disubstituted 1,2,3-triazole comprising:

contacting a human blood plasma solution of an organic azide and a terminal alkyne with a source of catalytic Cu(I) ion to form by cycloaddition a 1,4-disubstituted 1,2,3-triazole.

2. The process of claim 1 wherein the solution further comprises at least one ligand comprising at least one functional group selected from the group consisting of a nitrile, an isonitrile, a primary amine, a secondary amine, a tertiary amine, a nitrogen bearing heterocycle, a carboxylate, a halide, an alcohol, a thiol, a sulfide, a phosphine, and a phosphite.

3. The process of claim 1 wherein the solution further comprises at least one polyvalent ligand comprising one or more functional groups selected from the group consisting of a nitrile, an isonitrile, a primary amine, a secondary amine, a tertiary amine, a nitrogen bearing heterocycle, a carboxylate, a halide, an alcohol, a thiol, a sulfide, a phosphine, and a phosphite.

4. The process of claim 1 wherein the source of catalytic Cu(I) ion comprises a Cu(I) salt.

5. The process of claim 1 wherein the source of catalytic Cu(I) comprises Cu(II) ion in combination with a reducing agent.

6. The process of claim 1 wherein the source of catalytic Cu(I) comprises copper metal.

7. A copper catalyzed process for preparing a 1,4-disubstituted 1,2,3-triazole comprising:

contacting an aqueous solution of an organic azide and a terminal alkyne with a source of Cu(I) ion and a ligand for Cu(I) to form a 1,4-disubstituted 1,2,3-triazole, wherein the aqueous solution comprises water and a cosolvent.

8. The process of claim 7 wherein the cosolvent comprises a nitrile.

9. The process of claim 8 wherein the nitrile comprises acetonitrile.

10. The process of claim 1 wherein the cosolvent comprises an alcohol.

11. The process of claim 10 wherein the alcohol comprises ethanol or tert-butanol.

12. The process of claim 7 wherein the ligand comprises one or more functional groups selected from the group consisting of a nitrile, an isonitrile, a primary amine, a secondary amine, a tertiary amine, a nitrogen bearing heterocycle, a carboxylate, a halide, an alcohol, a thiol, a sulfide, a phosphine, and a phosphite.

13. The process of claim 7 wherein the source of Cu(I) ion comprises a Cu(I) salt.

14. The process of claim 7 wherein the source of catalytic Cu(I) comprises Cu(II) ion in combination with a reducing agent.

15. The process of claim 14 wherein the reducing agent comprises ascorbate.

16. The process of claim 14 wherein the Cu(II) ion is provided as a Cu(II) salt.

17. The process of claim 14 wherein the Cu(II) salt comprises CuSO 4 or a hydrate thereof.

18. The process of claim 7 wherein the source of catalytic Cu(I) comprises copper metal.

19. A copper catalyzed process for preparing a 1,4-disubstituted 1,2,3-triazole comprising:

contacting an aqueous solution of an organic azide and a terminal alkyne with a source of Cu(I) ion and a ligand for Cu(I) to form a 1,4-disubstituted 1,2,3-triazole, wherein the aqueous solution comprises water and a cosolvent comprising ethanol, acetonitrile, or a combination thereof; and the source of Cu(I) ion comprises a Cu(II) salt and ascorbate.

20. The process of claim 19 wherein the ligand comprises one or more functional groups selected from the group consisting of a nitrile, an isonitrile, a primary amine, a secondary amine, a tertiary amine, a nitrogen bearing heterocycle, a carboxylate, a halide, an alcohol, a thiol, a sulfide, a phosphine, and a phosphite.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 14, 2019
From: CEMPRA PHARMACEUTICALS, INC.
To: TETARD, INC.
Reel/Frame 050056/0731 →
CONFIRMATORY LICENSE Recorded Dec 21, 2017
From: SCRIPPS RESEARCH INSTITUTE
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 044932/0252 →