IP Library Granted Patent US 12,240,810
Granted Patent B2
US 12,240,810 · App. 17/428,070 · Granted Mar 4, 2025

Chiral-substituted poly-N-vinylpyrrolidinones and complexes with bimetallic nanoclusters and uses thereof in asymmetric oxidation reactions

Inventor: Duy H. Hua (Manhattan, KS)
Assignee: Kansas State University Research
C07D205/08B01J35/50C07D207/28C07D211/78C07D305/12C07D307/33C07D309/30C07D471/04C07D471/22C07D487/04C07J1/00C08F126/10C08F226/10B82Y30/00B82Y40/00
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Quick Facts
Patent No.
US 12,240,810
App. No.
17/428,070
Granted
Mar 4, 2025
Kind
B2
Abstract

Chiral polyvinylpyrrolidinone (CSPVP), complexes of CSPVP with a core species, such as a bimetallic nanocluster catalyst, and enantioselective oxidation reactions utilizing such complexes are disclosed. The catalytic complexes have exhibited the ability to achieve reaction products have a very high degree of optical purifies. These reaction products can be used as reagents in the synthesis of complex organic molecules, such as bioactive products, and C—H bond oxidation of complex molecules including various drugs and natural products.

Claims (35)

1. A chiral substituted polyvinylpyrrolidinone compound having the formula

wherein each R is individually selected from the group consisting of OH and C1-C30 aliphatic and aromatic functional groups, and n is greater than 50.

2. The compound of claim 1 , wherein at least two R groups are identical.

3. The compound of claim 1 , wherein the compound has the formula

4. The compound of claim 1 , wherein the compound has the formula

5. The compound of claim 1 , wherein each R group is selected from the group consisting of ethers, aliphatic hydrocarbons, and aromatic hydrocarbons.

6. The compound of claim 1 , wherein each R group is selected from the group consisting of CH 3 , CH 2 CH 3 , CH(CH 3 ) 2 , CH (cyclohexyl) 2 , Ph, CH 2 Ph, CH 2 O-t-Bu, CH 2 (1-Naph), CH 2 OH, and CH 2 OCHPh 2 .

7. The compound of claim 1 , wherein the compound comprises

8. The compound of claim 1 , wherein the compound has a molecular weight of at least 50,000 g/mol and wherein n is from 50 to about 500.

9. A complex comprising the chiral substituted polyvinylpyrrolidinone compound of claim 1 bound to a core species selected from the group consisting of nanoparticulate materials, proteins, DNA, siRNA, and dsRNA.

10. The complex of claim 9 , wherein the complex comprises a nanoparticle cluster, and wherein the nanoparticle cluster comprises one or more metals selected from the group consisting of Au, Pd, Cu, Rh, Ce, Mo, Ni, Ru, W, and Fe.

11. The complex of claim 1 , wherein the nanoparticle cluster is bimetallic and is selected from the group consisting of Pd/Au, Cu/Au, Rh/Au, Ce/Au, Mo/Au, W/Au, Ru/Au, and Fe/Au.

12. The complex of claim 9 , wherein the chiral substituted polyvinylpyrrolidinone compound encapsulates the core species.

13. A method of asymmetrically oxidizing organic molecules comprising reacting the organic molecule with one or more reagents in the presence of a complex comprising the chiral substituted polyvinylpyrrolidinone compound of claim 1 bound to a metallic nanocluster to produce chiral molecules.

14. The method of claim 13 , wherein the organic molecule is an alkene or cycloalkane, and the reaction results in the oxidation of a carbon-carbon double bond producing chiral diols.

15. The method of claim 13 , wherein the organic molecule is an alkane or cycloalkane, and the reaction oxidizes a carbon-hydrogen bond in the alkane or cycloalkane to form a chiral alcohol or ketone molecule possessing a hydroxyl or carbonyl functional group.

16. The method of claim 13 , wherein the organic molecule comprises an alkene, and the reaction comprises a ring-closing reaction resulting in the formation of a lactone or lactam.

17. The method of claim 13 , wherein the reaction generates a reaction product comprising two enantiomers, and wherein the enantiomeric excess of one of the enantiomers is greater than 50%.

18. The method of claim 17 , wherein the reaction generates a reaction product that is enantiopure.

19. The method of claim 13 , wherein the reaction generates a reaction product having a hydroxyl or ketone functional group, and wherein the reaction product is further reacted with an organic compound in which the organic compound is added to the reaction product at the site of the hydroxyl or ketone functional group.

20. The method of claim 13 , wherein the nanocluster comprises one or more metals selected from the group consisting of Au, Pd, Cu, Rh, Ce, Mo, Ni, Ru, W, and Fe.

21. The method of claim 20 , wherein the nanocluster is bimetallic and is selected from the group consisting of Pd/Au, Cu/Au, Rh/Au, Ce/Au, Mo/Au, Ni/Au, W/Au, Ru/Au, and Fe/Au.

22. A compound produced by reacting a substrate with one or more reagents in the presence of a complex comprising the chiral substituted polyvinylpyrrolidinone compound of claim 1 bound to a metallic nanocluster.

23. The compound of claim 22 , wherein the compound comprises an enantiomeric excess of greater than 80% without having undergone a separate separation step to isolate a particular enantiomer.

24. A method of synthesizing the chiral substituted polyvinylpyrrolidinone compound of claim 1 from D-isoascorbic acid comprising:

converting the isoascorbic acid to a pyrrolidinone through a sequence of (i) oxidative cleavage of the isoascorbic acid to produce a D-erthronolactone, (ii) ketalization of the D-erthronolactone to produce a ketalized lactone, (iii) S N 2-type ring opening of the ketalized lactone, and (iv) reduction of an azido functional group;

converting the pyrrolidinone to an N-vinylpyrrolidinone through an N-vinylation reaction; and

polymerizing the N-vinylpyrrolidinone to form the chiral substituted polyvinylpyrrolidinone compound of claim 1 .

25. A method of synthesizing the chiral substituted polyvinylpyrrolidinone compound of claim 1 from D-ribose comprising

converting the D-ribose into an acetonide sugar;

reacting the acetonide sugar to produce a lactol;

oxidizing the lactol with pyridinium chlorochromate to produce a lactone;

reacting the lactone with dimethylformamide to produce a pyrrolidinone;

converting the pyrrolidinone to an N-vinylpyrrolidinone through an N-vinylation reaction; and

polymerizing the N-vinylpyrrolidinone to form the chiral substituted polyvinylpyrrolidinone compound of claim 1 .

Assignments (2)
CONFIRMATORY LICENSE Recorded Apr 9, 2025
From: KANSAS STATE UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 070794/0102 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 4, 2021
From: HUA, DUY H.
To: KANSAS STATE UNIVERSITY RESEARCH FOUNDATION
Reel/Frame 057075/0750 →
Continuity (2)
Provisional Application 62800823 · Feb 4, 2019
Related Publication 20220204447A1 · Jun 30, 2022
References Cited (7)
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Hao, et al., “Chiral Substituted Poly-N-vinylpyrrolidinones and Bimetallic Nanoclusters in Catalytic Asymmetric Oxidation Reactions”, J Am Chem Soc, 2016, 138(51), pp. 16839-16848. [cited by applicant]
Dinari, et al., “Ultrasound-assisted one-pot preparation of organo-modified nano-sized layered double hydroxide and its nanocomposites with polyvinylpyrrolidone”, J Polym Res, 2014, 21, 8 pages. [cited by applicant]