IP Library Granted Patent US 11,649,240
Granted Patent B2
US 11,649,240 · App. 17/099,231 · Granted May 16, 2023

Substituted 4-phenylpiperidines, their preparation and use

Inventors: Konstantin Petrukhin (New Windsor, NY); Christopher Cioffi (Troy, NY); Graham Johnson (Sanbornton, NH); Rando Allikmets (Cornwall on Hudson, NY); Emily Freeman (Voorheesville, NY); Ping Chen (Slingerlands, NY); Michael Conlon (Schenectady, NY); Lei Zhu (Glenmont, NY)
Assignee: THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK
C07D487/04C07D471/04
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Quick Facts
Patent No.
US 11,649,240
App. No.
17/099,231
Granted
May 16, 2023
Kind
B2
Abstract

The present invention provides a compound having the structure: wherein R 1 , R 2 , R 3 , R 4 , and R 5 are each independently H, halogen, CF 3 or C 1 -C 4 alkyl, wherein two or more of R 1 , R 2 , R 3 , R 4 , or R 5 are other than H; R 6 is H, OH, or halogen; and B is a substituted or unsubstituted heterobicycle, wherein when R 1 is CF 3 , R 2 is H, R 3 is F, R 4 is H, and R 5 is H, or R 1 is H, R 2 is CF 3 , R 3 is H, R 4 is CF 3 , and R 5 is H, or R 1 is Cl, R 2 is H, R 3 is H, R 4 is F, and R 5 is H, or R 1 is CF 3 , R 2 is H, R 3 is F, R 4 is H, and R 5 is H, or R 1 is CF 3 , R 2 is F, R 3 is H, R 4 is H, and R 5 is H, or R 1 is Cl, R 2 is F, R 3 is H, R 4 is H, and R 5 is H, then B is other than or a pharmaceutically acceptable salt thereof.

Claims (36)

1. A method for the preparation of Compound 81:

by conversion from Compound 33:

2. The method of claim 1 comprising treatment of Compound 33:

with an acid, followed by coupling with an acid chloride.

3. The method of claim 2 , wherein the acid is trifluoroacetic acid.

4. The method of claim 1 comprising treatment of Compound 34:

with an acid chloride.

5. The method of claim 2 , wherein the method comprises treatment with trifluoroacetic acid in methylene chloride followed by coupling with acetyl chloride.

6. The method of claim 1 , wherein compound 81 is purified by chromatography.

7. The method of claim 1 , wherein the method further comprises forming a pharmaceutical composition of compound 81, wherein the pharmaceutical composition comprises a pharmaceutically acceptable carrier.

8. The method of claim 1 , wherein Compound 33 is prepared by reacting 4-(3,4-difluoro-2-(trifluoromethyl)phenyl)piperidine:

with 6-(tert-butoxycarbonyl)-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carboxylic acid:

under coupling conditions.

9. The method of claim 8 , wherein 4-(3,4-difluoro-2-(trifluoromethyl)phenyl)piperidine:

is prepared from Compound 8:

and an acid.

10. The method of claim 9 , wherein the acid is trifluoroacetic acid.

11. The method of claim 9 , wherein 4-(3,4-difluoro-2-(trifluoromethyl)phenyl)piperidine:

is prepared from Compound 6:

12. A method for the preparation of Compound 65:

by conversion from 6-bromo-[1,2,4]triazolo[4,3-a]pyridine-3-carboxylate:

13. The method of claim 11 comprising treatment of Compound 5:

with lithium 6-bromo-[1,2,4]triazolo[4,3-a]pyridine-3-carboxylate:

under coupling conditions.

14. The method of claim 12 comprising treatment of 6-bromo-[1,2,4]triazolo[4,3-a]pyridine-3-carboxylic acid:

with lithium hydroxide.

15. The method of claim 11 comprising treatment of (6-bromo-[1,2,4]triazolo[4,3-a]pyridin-3-yl) (4-(3-fluoro-2-(trifluoromethyl)phenyl)piperidin-1-yl)methanone:

with zinc cyanide and a palladium catalyst.

16. The method of claim 11 , wherein Compound 65 is purified by chromatography.

17. The method of claim 11 , wherein the method further comprises forming a pharmaceutical composition of Compound 65, wherein the pharmaceutical composition comprises a pharmaceutically acceptable carrier.

18. The method of claim 11 , wherein Compound 5:

is prepared from Compound 4:

and an acid.

19. The method of claim 18 , wherein the acid is trifluoroacetic acid.

20. The method of claim 18 , wherein Compound 5:

is prepared from Compound 1:

Assignments (3)
CONFIRMATORY LICENSE Recorded Oct 26, 2023
From: COLUMBIA UNIV NEW YORK MORNINGSIDE
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 065369/0430 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 17, 2020
From: PETRUKHIN, KONSTANTIN; JOHNSON, GRAHAM; ALLIKMETS, RANDO
To: THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK
Reel/Frame 054389/0875 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 17, 2020
From: CIOFFI, CHRISTOPHER; FREEMAN, EMILY; CHEN, PING; CONLON, MICHAEL; ZHU, LEI
To: THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK
Reel/Frame 054449/0286 →
Continuity (7)
Continuation 16520886 · Jul 24, 2019
Continuation 16058299 · Aug 8, 2018
Continuation 15722760 · Oct 2, 2017
Continuation 15254966 · Sep 1, 2016
Continuation 14699672 · Apr 29, 2015
Provisional Application 61986578 · Apr 30, 2014
Related Publication 20210214360A1 · Jul 15, 2021
Cited By (2)
US 12,404,277 US 12,440,486