IP Library Granted Patent US 7,053,236
Granted Patent B2
US 7,053,236 · App. 10/460,051 · Granted May 30, 2006

Catalytic asymmetric desymmetrization of prochiral and meso compounds

Assignee: Brandeis University
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Quick Facts
Patent No.
US 7,053,236
App. No.
10/460,051
Granted
May 30, 2006
Kind
B2
Abstract

The present invention relates to methods for the synthesis of chiral non-racemic products, e.g., enantiomerically-enriched hemiesters, from prochiral and meso starting materials, e.g., prochiral and meso cyclic anhydrides. The present invention also relates to catalysts for the aforementioned methods, and methods for synthesizing these catalysts.

Claims (29)

1. A method of preparing a chiral, non-racemic compound from a prochiral substituted cyclic anhydride or a meso substituted cyclic anhydride, comprising the step of:

reacting a prochiral substituted cyclic anhydride or a meso substituted cyclic anhydride with a nucleophile in the presence of a chiral, non-racemic tertiary amine catalyst; wherein said prochiral substituted cyclic anhydride or said meso substituted cyclic anhydride comprises an internal plane of symmetry or point of symmetry or both; wherein said meso substituted cyclic anhydride comprises at least two chiral centers; and wherein said nucleophile is an alcohol, thiol or amine; thereby producing a chiral, non-racemic compound.

2. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or a substituted glutaric anhydride.

3. The method of claim 1 , wherein said nucleophile is an alcohol.

4. The method of claim 1 , wherein said nucleophile is a primary alcohol.

5. The method of claim 1 , wherein said nucleophile is methanol or CF 3 CH 2 OH.

6. The method of claim 1 , wherein said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP, QD-TB, (DHQ) 2 PHAL, (DHQD) 2 PHAL, (DHQ) 2 PYR, (DHQD) 2 PYR, (DHQ) 2 AQN, (DHQD) 2 AQN, DHQ-CLB, DHQD-CLB, DHQ-MEQ, DHQD-MEQ, DHQ-AQN, DHQD-AQN, DHQ-PHN, or DHQD-PHN.

7. The method of claim 1 , wherein said chiral, non-racemic tertiary amine catalyst is DHQD-PHN or (DHQD) 2 AQN.

8. The method of claim 1 , wherein said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP or QD-TB.

9. The method of claim 1 , wherein said chiral, non-racemic tertiary amine catalyst is QD-PP.

10. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is an alcohol; and said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP, QD-TB, (DHQ) 2 PHAL, (DHQD) 2 PHAL, (DHQ) 2 PYR, (DHQD) 2 PYR, (DHQ) 2 AQN, (DHQD) 2 AQN, DHQ-CLB, DHQD-CLB, DHQ-MEQ, DHQD-MEQ, DHQ-AQN, DHQD-AQN, DHQ-PHN, or DHQD-PHN.

11. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is a primary alcohol; and said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP, QD-TB, (DHQ) 2 PHAL, (DHQD) 2 PHAL, (DHQ) 2 PYR, (DHQD) 2 PYR, (DHQ) 2 AQN, (DHQD) 2 AQN, DHQ-CLB, DHQD-CLB, DHQ-MEQ, DHQD-MEQ, DHQ-AQN, DHQD-AQN, DHQ-PHN, or DHQD-PHN.

12. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is methanol or CF 3 CH 2 OH; and said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP, QD-TB, (DHQ) 2 PHAL, (DHQD) 2 PHAL, (DHQ) 2 PYR, (DHQD) 2 PYR, (DHQ) 2 AQN, (DHQD) 2 AQN, DHQ-CLB, DHQD-CLB, DHQ-MEQ, DHQD-MEQ, DHQ-AQN, DHQD-AQN, DHQ-PHN, or DHQD-PHN.

13. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is an alcohol; and said chiral, non-racemic tertiary amine catalyst is DHQD-PHN or (DHQD) 2 AQN.

14. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is a primary alcohol; and said chiral, non-racemic tertiary amine catalyst is DHQD-PHN or (DHQD) 2 AQN.

15. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is methanol or CF 3 CH 2 OH; and said chiral, non-racemic tertiary amine catalyst is DHQD-PHN or (DHQD) 2 AQN.

16. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is an alcohol; and said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP or QD-TB.

17. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is a primary alcohol; and said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP or QD-TB.

18. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is methanol or CF 3 CH 2 OH; and said chiral, non-racemic tertiary amine catalyst is Q-PP, Q-TB, QD-PP or QD-TB.

19. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is an alcohol; and said chiral, non-racemic tertiary amine catalyst is QD-PP.

20. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is a primary alcohol; and said chiral, non-racemic tertiary amine catalyst is QD-PP.

21. The method of claim 1 , wherein said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride is a substituted succinic anhydride or substituted glutaric anhydride; said nucleophile is methanol or CF 3 CH 2 OH; and said chiral, non-racemic tertiary amine catalyst is QD-PP.

22. The method of claim 1 , wherein said chiral, non-racemic tertiary amine catalyst is present in less than about 30 mol % relative to said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride.

23. The method of claim 1 , wherein said chiral, non-racemic tertiary amine catalyst is present in less than about 20 mol % relative to said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride.

24. The method of claim 1 , wherein said chiral, non-racemic tertiary amine catalyst is present in less than about 10 mol % relative to said prochiral substituted cyclic anhydride or meso substituted cyclic anhydride.

25. The method of claim 1 , wherein said chiral, non-racemic compound has an enantiomeric excess greater than about 50%.

26. The method of claim 1 , wherein said chiral, non-racemic compound has an enantiomeric excess greater than about 70%.

27. The method of claim 1 , wherein said chiral, non-racemic compound has an enantiomeric excess greater than about 90%.

28. The method of claim 1 , wherein said chiral, non-racemic compound has an enantiomeric excess greater than about 95%.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jan 19, 2022
From: BRANDEIS UNIVERSITY
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 058772/0290 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 16, 2004
From: DENG, LI; CHEN, YONGGANG; TIAN, SHIKAI
To: BRANDEIS UNIVERSITY
Reel/Frame 014896/0552 →
Continuity (4)
Continuation In Part 1036658100 · Feb 13, 2003
Continuation 0982516700 · Apr 3, 2001
Provisional Application 6019452000 · Apr 4, 2000
Related Publication 20040082809A1 · Apr 29, 2004