IP Library Granted Patent US 9,868,755
Granted Patent B2
US 9,868,755 · App. 15/219,755 · Granted Jan 16, 2018

Reagent-controlled stereoselective glycosylation

Inventors: Clay S. Bennett (Somerville, MA); John P. Issa (Medford, MA); Dina Lloyd (Concord, NH)
Assignee: Trustees of Tufts College
C07H19/01C07H1/00C07H3/04C07H5/10C07H9/04C07H13/00C07H15/14C07H15/18C07H15/203C07B2200/07
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Quick Facts
Patent No.
US 9,868,755
App. No.
15/219,755
Granted
Jan 16, 2018
Kind
B2
Abstract

Provided are methods for the efficient stereoselective formation of glycosidic bonds, without recourse to prosthetic or directing groups.

Claims (31)

1. A method of forming a glycosidic bond, comprising:

combining a first solvent, a reducing sugar, and a first strong Bronsted base, thereby forming a first reaction mixture;

combining a sulfonylating agent and the first reaction mixture, thereby forming a glycosyl sulfonate;

combining a second solvent, a glycosyl acceptor, and a second strong Bronsted base, thereby forming a second reaction mixture; and

combining the glycosyl sulfonate and the second reaction mixture, thereby forming a glycosidic bond;

wherein the reducing sugar is a pyranose; the sulfonylating agent is a sulfonyl halide; and

the glycosidic bond is formed with greater than or equal to 90% stereoselectivity for a β linkage.

2. The method of claim 1 , wherein the glycosidic bond is formed with greater than or equal to 95% stereoselectivity for a β linkage.

3. The method of claim 1 , wherein the reducing sugar is a 2-deoxy-sugar.

4. The method of claim 1 , wherein the reducing sugar is a D -sugar.

5. The method of claim 4 , wherein the reducing sugar is a 2-deoxy- D -sugar.

6. The method of claim 4 , wherein the reducing sugar is a D -pyranose.

7. The method of claim 1 , wherein the reducing sugar is an L -sugar.

8. The method of claim 7 , wherein the reducing sugar is a 2-deoxy- L -sugar.

9. The method of claim 7 , wherein the reducing sugar is an L -pyranose.

10. The method of claim 1 , wherein the reducing sugar is a 2,6-dideoxy- L -sugar.

11. The method of claim 1 , wherein the reducing sugar is selected from the group consisting of:

12. The method of claim 1 , wherein the first strong Bronsted base is non-nucleophilic.

13. The method of claim 1 , wherein the second strong Bronsted base is non-nucleophilic.

14. The method of claim 1 , wherein the first strong Bronsted base is non-nucleophilic; and the second strong Bronsted base is non-nucleophilic.

15. The method of claim 1 , wherein the first strong Bronsted base is selected from the group consisting of: alkali metal alkoxides, alkali metal amides, alkaline earth metal alkoxides, and alkaline earth metal amides.

16. The method of claim 1 , wherein the first strong Bronsted base is selected from the group consisting of: sodium tert-butoxide, potassium tert-butoxide, lithium tert-butoxide, lithium diisopropylamide, lithium tetramethylpiperidide, sodium hexamethyldisilazane (NaHMDS), and potassium hexamethyldisilazane (KHMDS).

17. The method of claim 1 , wherein the first strong Bronsted base is potassium hexamethyldisilazane (KHMDS).

18. The method of claim 1 , wherein the second strong Bronsted base is selected from the group consisting of: alkali metal alkoxides, alkali metal amides, alkaline earth metal alkoxides, and alkaline earth metal amides.

19. The method of claim 1 , wherein the second strong Bronsted base is selected from the group consisting of: sodium tert-butoxide, potassium tert-butoxide, lithium tert-butoxide, lithium diisopropylamide, lithium tetramethylpiperidide, sodium hexamethyldisilazane (NaHMDS), and potassium hexamethyldisilazane (KHMDS).

20. The method of claim 1 , wherein the second strong Bronsted base is potassium hexamethyldisilazane (KHMDS).

21. The method of claim 1 , wherein the first strong Bronsted base is same as the second strong Bronsted base.

22. The method of claim 1 , wherein the first reaction mixture further comprises tri-tert-butylpyrimidine (TTBP).

23. The method of claim 1 , wherein the glycosyl acceptor comprises an alcohol, a thiol, or an amine.

24. The method of claim 1 , wherein the glycosyl acceptor is a monosaccharide, a disaccharide, an oligosaccharide, or a polysaccharide, each comprising at least one —OH, —SH, or primary or secondary amino group.

25. The method of claim 1 , wherein the glycosyl acceptor is selected from the group consisting of: PhSH, t-BuSH, 2-naphthol, 1-naphthol, phenol, o-cresol, p-methoxyphenol, p-trifluoromethylphenol,

Assignments (2)
CONFIRMATORY LICENSE Recorded Mar 29, 2017
From: TUFTS UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 041784/0637 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 26, 2016
From: BENNETT, CLAY S.; ISSA, JOHN PAUL; LLOYD, DINA
To: TRUSTEES OF TUFTS COLLEGE
Reel/Frame 039260/0316 →
Continuity (5)
Continuation 14445917 · Jul 29, 2014
Provisional Application 61946289 · Feb 28, 2014
Provisional Application 61886915 · Oct 4, 2013
Provisional Application 61860010 · Jul 30, 2013
Related Publication 20170051003A1 · Feb 23, 2017