IP Library Granted Patent US 10,543,481
Granted Patent B2
US 10,543,481 · App. 15/019,673 · Granted Jan 28, 2020

Targeted, metal-catalyzed fluorination of complex compounds with fluoride ion via decarboxylation

Inventors: John T. Groves (Princeton, NJ); Xiongyi Huang (Plainsboro, NJ)
Assignee: TRUSTEES OF PRINCETON UNIVESITY
B01J31/183A61K51/0423A61K51/0446A61K51/0455A61K51/0493C07C41/22C07C49/80C07D209/48C07D213/643C07D319/20B01J2231/40B01J2531/72
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Quick Facts
Patent No.
US 10,543,481
App. No.
15/019,673
Granted
Jan 28, 2020
Kind
B2
Abstract

Methods of preparing fluorinated compounds by carboxylative fluorination using fluoride are contained herein. Fluorinated compounds are provided. Methods of using fluorinated compounds are contained herein.

Claims (8)

1. A method of targeted fluorination of a compound containing a carboxyl group, the method comprising combining the compound, a nucleophilic fluoride source comprising a fluorine moiety, a manganese catalyst, a solvent and an iodine(III) oxidant, wherein the iodine (III) oxidant is selected from the group consisting of dichlorobenzene, iodobenzene diacetate, Bis(tert-butylcarbonyloxy)iodobenzene, iodosylmesitylene, [Bis(trifluoroacetoxy)iodo]benzene, [hydroxyl(tosyloxy)iodo]benzene, iodomesitylene diacetate, Iodosylpentafluorobenzene, [Bis(trifluoroacetoxy)iodo] pentafluorobenzene, 3,3-dimethyl-1-fluoro, 1, 2-benziodoxole, and (2-tert-butylsulfonyl)iodosobenzene and the carboxyl group is replaced by the fluorine moiety.

2. The method of claim 1 , wherein the manganese catalyst is a manganese porphyrin or a manganese salen.

3. The method of claim 1 , wherein the nucleophilic fluoride source is trialkyl amine trihydrofluoride.

4. The method of claim 3 , wherein the nucleophilic fluorides source is triethylamine trihydrofluoride.

5. The method of claim 1 , wherein combining comprises: mixing the manganese catalyst, the nucleophilic fluoride source, the compound and the solvent under an inert atmosphere to form a first mixture; and adding the iodine (III) oxidant to the first mixture to form a second mixture.

6. The method of claim 5 further comprising maintaining the first mixture at a temperature from 25° C. to 80° C.

7. The method of claim 5 , wherein the step of adding the oxidant occurs over a period of 45 minutes to 90 minutes.

8. The method of claim 1 , wherein combining further comprises adding benzoic acid.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jan 5, 2017
From: PRINCETON UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 041257/0244 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 5, 2016
From: GROVES, JOHN T.; HUANG, XIONGYI
To: TRUSTEES OF PRINCETON UNIVERSITY
Reel/Frame 038476/0507 →
Continuity (6)
Continuation In Part 14239719
Provisional Application 62113847 · Feb 9, 2015
Provisional Application 61525301 · Aug 19, 2011
Provisional Application 61639523 · Apr 27, 2012
Provisional Application 61679367 · Aug 3, 2012
Related Publication 20160158388A1 · Jun 9, 2016