IP Library Granted Patent US 9,708,269
Granted Patent B2
US 9,708,269 · App. 15/073,251 · Granted Jul 18, 2017

Process for making isoquinoline compounds

Inventors: Michael D. Thompson (Redwood City, CA); Jung Min Park (San Francisco, CA); Michael P. Arend (Foster City, CA)
Assignee: FibroGen, Inc.
C07D217/26
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Quick Facts
Patent No.
US 9,708,269
App. No.
15/073,251
Granted
Jul 18, 2017
Kind
B2
Abstract

The present invention relates to methods for making isoquinoline compounds and the intermediate compounds achieved thereby. Such compounds can be used to prepare compounds and compositions capable of decreasing HIF hydroxylase enzyme activity, thereby increasing the stability and/or activity of hypoxia inducible factor (HIF).

Claims (51)

1. A compound of formula VIII:

wherein:

Z is O, NR 1 , or S;

R 1 is selected from the group consisting of hydrogen and alkyl;

R 2 is selected from the group consisting of hydrogen and alkyl which is unsubstituted or substituted with one or more substituents independently selected from the group consisting of cycloalkyl, heterocyclyl, aryl, and heteroaryl;

R 3 and R 4 are independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, substituted heteroaryl, halo, hydroxy, cyano, —S(O) n —N(R 8 )—R 8 , where n is 0, 1, or 2, —NR 8 C(O)NR 8 R 8 , and —X 1 R 8 where X 1 is oxygen, —S(O) n —, or —NR 9 — where n is 0, 1, or 2, or R 3 , R 4 together with the carbon atom pendent thereto, form a cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, or substituted heteroaryl;

R 5 and R 6 are independently selected from the group consisting of hydrogen, halo, alkyl, substituted alkyl, alkoxy, substituted alkoxy, aryl, substituted aryl, heteroaryl, substituted heteroaryl, and —X 2 R 10 where X 2 is oxygen, —S(O) n —, or —NR 13 — where n is 0, 1, or 2, or when X 2 is —NR 13 —, then R 13 and R 10 , together with the nitrogen atom to which they are bound, can be joined to form a heterocyclyl or substituted heterocyclyl group;

R 7 is either —N(R 11 )(R 11 ) or —OC(O)R 12 ;

each R 8 is independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, aryl, substituted aryl, cycloalkyl, substituted cycloalkyl, heteroaryl, substituted heteroaryl, heterocyclyl, and substituted heterocyclyl provided that when X 1 is —SO— or —SO 2 —, then R 8 is not hydrogen;

R 9 and R 13 are independently selected from the group consisting of hydrogen, alkyl, and aryl;

R 10 is selected from the group consisting of alkyl, substituted alkyl, aryl, substituted aryl, heteroaryl, substituted heteroaryl, heterocyclyl, and substituted heterocyclyl;

each R 11 is independently selected from alkyl, benzyl, or aryl, or two R 11 together with the nitrogen atom to which they are attached form a 4-8 membered heterocyclyl or a heteroaryl; and

R 12 is selected from the group consisting of alkyl, aryl, heteroaryl, and heterocyclyl;

or a salt, ester, stereoisomer, or mixture of stereoisomers thereof;

provided that the compound is not 1-dimethylaminomethyl-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester.

2. A compound of formula VIIIA:

wherein:

R 2 is selected from the group consisting of hydrogen and alkyl which is unsubstituted or substituted with one or more substituents independently selected from the group consisting of cycloalkyl, heterocyclyl, aryl, and heteroaryl;

R 3 and R 4 are independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, substituted heteroaryl, halo, hydroxy, cyano, —S(O) n —N(R 8 )—R 8 where n is 0, 1, or 2, —NR 8 C(O)NR 8 R 8 , and —X 1 R 8 where X 1 is oxygen, —S(O) n —, or —NR 9 — where n is 0, 1, or 2, or R 3 , R 4 together with the carbon atom pendent thereto, form a cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, or substituted heteroaryl;

R 5 and R 6 are independently selected from the group consisting of hydrogen, halo, alkyl, substituted alkyl, alkoxy, substituted alkoxy, aryl, substituted aryl, heteroaryl, substituted heteroaryl, and —X 2 R 10 where X 2 is oxygen, —S(O) n —, or —NR 13 — where n is 0, 1, or 2, or when X 2 is —NR 13 —, then R 13 and R 10 , together with the nitrogen atom to which they are bound, can be joined to form a heterocyclyl or substituted heterocyclyl group;

R 7 is either —N(R 11 )(R 11 ) or —OC(O)R 12 ;

each R 8 is independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, aryl, substituted aryl, cycloalkyl, substituted cycloalkyl, heteroaryl, substituted heteroaryl, heterocyclyl and substituted heterocyclyl provided that when X 1 is —SO— or —SO 2 —, then R 8 is not hydrogen;

R 9 and R 13 are independently selected from the group consisting of hydrogen, alkyl, and aryl;

R 10 is selected from the group consisting of alkyl, substituted alkyl, aryl, substituted aryl, heteroaryl, substituted heteroaryl, heterocyclyl, and substituted heterocyclyl;

each R 11 is independently selected from alkyl, benzyl, or aryl, or two R 11 together with the nitrogen atom to which they are attached form a 4-8 membered heterocyclyl or a heteroaryl; and

R 12 is selected from the group consisting of alkyl, aryl, heteroaryl, and heterocyclyl;

or a salt, ester, stereoisomer, or mixture of stereoisomers thereof;

provided that the compound is not 1-dimethylaminomethyl-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester.

3. The compound of claim 1 or claim 2 , wherein R 2 is unsubstituted alkyl.

4. The compound of claim 1 or claim 2 , wherein R 5 and R 6 are hydrogen.

5. The compound of claim 1 or claim 2 , wherein:

R 2 is selected from the group consisting of alkyl which is unsubstituted or substituted with one or more substituents independently selected from the group consisting of cycloalkyl, heterocyclyl, aryl, and heteroaryl; and

R 5 and R 6 are hydrogen.

6. The compound of claim 1 or claim 2 , wherein R 7 is —N(R 11 )(R 11 ) and R 11 is C 1 to C 4 alkyl.

7. The compound of claim 1 or claim 2 , wherein R 7 is —OC(O)R 12 and R 12 is C 1 to C 4 alkyl.

8. The compound of claim 1 or claim 2 , wherein:

R 2 is alkyl which is unsubstituted or substituted with one or more substituents independently selected from the group consisting of cycloalkyl, heterocyclyl, aryl, and heteroaryl;

R 3 and R 4 are independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, substituted heteroaryl, halo, hydroxy, cyano, —S(O) n —N(R 8 )—R 8 where n is 0, 1, or 2, —NR 8 C(O)NR 8 R 8 , and —X 1 R 8 where X 1 is oxygen, —S(O) n —, or —NR 9 — where n is 0, 1, or 2, or R 3 , R 4 together with the carbon atom pendent thereto, form a cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, or substituted heteroaryl;

R 5 and R 6 are hydrogen;

R 7 is —N(R 11 )(R 11 );

each R 8 is independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, aryl, substituted aryl, cycloalkyl, substituted cycloalkyl, heteroaryl, substituted heteroaryl, heterocyclyl, and substituted heterocyclyl provided that when X 1 is —SO— or —SO 2 —, then R 8 is not hydrogen;

R 9 is selected from the group consisting of hydrogen, alkyl, and aryl; and

each R 11 is independently selected from C 1 to C 4 alkyl or aryl.

9. The compound of claim 1 or claim 2 , wherein:

R 2 is alkyl which is unsubstituted or substituted with one or more substituents independently selected from the group consisting of cycloalkyl, heterocyclyl, aryl, and heteroaryl;

R 3 and R 4 are independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, substituted heteroaryl, halo, hydroxy, cyano, —S(O) n —N(R 8 )—R 8 where n is 0, 1, or 2, —NR 8 C(O)NR 8 R 8 , and —X 1 R 8 where X 1 is oxygen, —S(O) n —, or —NR 9 — where n is 0, 1, or 2, or R 3 , R 4 together with the carbon atom pendent thereto, form a cycloalkyl, substituted cycloalkyl, heterocyclyl, substituted heterocyclyl, aryl, substituted aryl, heteroaryl, or substituted heteroaryl;

R 5 and R 6 are hydrogen;

R 7 is —OC(O)R 12 ;

each R 8 is independently selected from the group consisting of hydrogen, alkyl, substituted alkyl, aryl, substituted aryl, cycloalkyl, substituted cycloalkyl, heteroaryl, substituted heteroaryl, heterocyclyl, and substituted heterocyclyl provided that when X 1 is —SO— or —SO 2 —, then R 8 is not hydrogen;

R 9 is selected from the group consisting of hydrogen, alkyl, and aryl; and

R 12 is selected from the group consisting of alkyl, aryl, heteroaryl, and heterocyclyl.

Assignments (4)
CHANGE OF NAME Recorded Feb 18, 2026
From: FIBROGEN, INC.
To: KYNTRA BIO, INC.
Reel/Frame 074923/0352 →
RELEASE OF SECURITY INTEREST Recorded Sep 3, 2025
From: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS AGENT
To: FIBROGEN, INC.
Reel/Frame 072785/0760 →
SECURITY INTEREST Recorded May 1, 2023
From: FIBROGEN, INC.
To: WILMINGTON TRUST, NATIONAL ASSOCIATION
Reel/Frame 063504/0221 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2016
From: THOMPSON, MICHAEL D.; PARK, JUNG MIN; AREND, MICHAEL P.
To: FIBROGEN, INC.
Reel/Frame 038515/0431 →
Continuity (3)
Continuation 14414879
Provisional Application 61672191 · Jul 16, 2012
Related Publication 20160194285A1 · Jul 7, 2016