IP Library Granted Patent US 10,137,209
Granted Patent B2
US 10,137,209 · App. 15/578,687 · Granted Nov 27, 2018

Gadolinium chelate compounds for use in magnetic resonance imaging

Inventors: Markus Berger (Berlin, DE); Jessica Lohrke (Berlin, DE); Christoph-Stephan Hilger (Berlin, DE); Gregor Jost (Berlin, DE); Thomas Frenzel (Berlin, DE); Detlev Suelzle (Berlin, DE); Johannes Platzek (Berlin, DE); Olaf Panknin (Berlin, DE); Hubertus Pietsch (Kleinmachnow, DE)
Assignee: BAYER PHARMA AKTIENGESELLSCHAFT
A61K49/106C07D257/02
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Quick Facts
Patent No.
US 10,137,209
App. No.
15/578,687
Granted
Nov 27, 2018
Kind
B2
Abstract

The present invention relates to a new class of high relaxivity extracellular gadolinium chelate complexes, to methods of preparing said compounds, and to the use of said compounds as MRI contrast agents.

Claims (96)

1. A compound of general formula (I), comprising 4, 5, 6, 7 or 8 gadolinium [4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl] groups,

in which:

represents a group selected from:

in which * on the A group indicates a point of attachment of the A group with R 1 ;

R 1 represents, independently from each other, a hydrogen atom or a substituent group selected from:

R 3 ,

in which * on the substituent group indicates a point of attachment of the substituent group with A group,

with the proviso that zero or only one of the R 1 groups present in the compound represent a hydrogen atom;

n represents an integer of 3 or 4;

R 2 represents, independently from each other, a hydrogen atom or a methyl group;

R 3 represents a group selected from:

in which * on the R 3 group indicates a point of attachment of the R 3 group with a nitrogen on the A group or the substituent group;

R 4 represents, independently from each other, a hydrogen atom or a methyl group; and

R 5 represents, independently from each other, a hydrogen atom or a methyl group;

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

2. The compound of claim 1 , wherein the compound comprises 4, 5, or 6 gadolinium [4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl] R 3 groups, and wherein:

represents a group selected from:

in which * on the A group indicates a point of attachment of the A group with R 1 .

3. The compound of claim 1 , wherein the compound comprises 4, 5, or 6 gadolinium [4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl] R 3 groups, and wherein:

represents a group selected from:

in which * on the A group indicates a point of attachment of the A group with R 1 ;

R 2 represents a hydrogen atom;

R 3 represents a group selected from:

in which * on the R 3 group indicates a point of attachment of the R 3 group with a nitrogen on the A group or the substituent group; and

R 4 represents a hydrogen atom;

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

4. The compound of claim 1 , wherein the compound comprises 4, 5, or 6 gadolinium [4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl] R 3 groups, and wherein:

represents a group selected from:

in which * on the A group indicates a point of attachment of the A group with R 1 ;

R 2 represents a hydrogen atom;

R 3 represents a group selected from:

in which * on the R 3 group indicates a point of attachment of the R 3 group with a nitrogen on the A group or the substituent group;

R 4 represents a hydrogen atom; and

R 5 represents a methyl group;

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

5. The compound of claim 1 , wherein the compound is selected from the group consisting of:

Tetragadolinium [4,10-bis(carboxylatomethyl)-7-{3,6,12,15-tetraoxo-16-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate,

Tetragadolinium {4,10-bis(carboxylatomethyl)-7-[(2R,16R)-3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({(2R)-2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate,

Tetragadolinium {4,10-bis(carboxylatomethyl)-7-[(2S,16S)-3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({(2S)-2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate,

Hexagadolinium 2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″,2″″″″″″,2′″″″″″″,2″″″″″″″, 2′″″″″″″″,2″″″″″″″″,2′″″″″″″″″-(1,4,7-triazonane-1,4,7-triyltris{carbonyl-1,4-diazepane-6,1,4-triylbis[(2-oxoethane-2,1-diyl)imino(1-oxopropane-1,2-diyl)-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]}) octadecaacetate,

Tetragadolinium 2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″-{1,4,7,10- tetraazacyclododecane-1,4,7,10-tetrayltetrakis[(2-oxoethane-2,1-diyl)imino(1-oxopropane-1,2-diyl)-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]}dodecaacetate,

Hexagadolinium 2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″,2″″″″″″,2′″″″″″″,2″″″″″″″, 2′″″″″″″″,2″″″″″″″″,2′″″″″″″″″-{3,7,10-triazatricyclo[3.3.3.0 1,5 ]undecane-3,7,10-triyltris[carbonyl-(3,6,11,14-tetraoxo-4,7,10,13-tetraazahexadecane-8,2,15-triyl)di-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]}octadecaacetate,

Tetragadolinium 2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″-(3,7,9-triazabicyclo-[3.3.1]nonane-3,7-diylbis{carbonyl-1,4-diazepane-6,1,4-triylbis[(2-oxoethane-2,1-diyl)-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]})dodecaacetate,

Tetragadolinium [4,10-bis(carboxylatomethyl)-7-{2,5,11,14-tetraoxo-15-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-8,8-bis({[({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)acetyl]amino}methyl)-3,6,10,13-tetraazapentadec-1-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate, and

Tetragadolinium {4,10-bis(carboxylatomethyl)-7-[2-oxo-2-({3-({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)-2,2-bis[({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)methyl]propyl}amino)ethyl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate,

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

6. The compound of claim 1 , wherein the compound is selected from the group consisting of:

Tetragadolinium [4,10-bis(carboxylatomethyl)-7-{3,6,12,15-tetraoxo-16-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate,

Tetragadolinium {4,10-bis(carboxylatomethyl)-7-[(2R,16R)-3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({(2R)-2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate,

Tetragadolinium {4,10-bis(carboxylatomethyl)-7-[(2S,16S)-3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({(2S)-2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate,

Tetragadolinium {4,10-bis(carboxylatomethyl)-7-[2-oxo-2-({3-({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)-2,2-bis[({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)methyl]propyl}amino)ethyl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate, and

Tetragadolinium [4,10-bis(carboxylatomethyl)-7-{2,5,11,14-tetraoxo-15-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-8,8-bis({[({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)acetyl]amino}methyl)-3,6,10,13-tetraazapentadec-1-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate,

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

7. A method of preparing a compound of general formula (I-d), the method comprising:

reacting a compound of formula 4,

in which has a structure:

where each group * represents a hydrogen atom or a salt thereof,

with a compound of general formula (III):

in which R 5 is a hydrogen atom or a methyl group, and LG represents an activating leaving group selected from the group consisting of pentafluorophenol, 4-nitrophenol, 1-hydroxypyrrolidine-2,5-dione, hydroxybenzotriazole, and 3H-[1,2,3]triazolo[4,5-b]pyridine-3-ol,

to afford a compound of general formula (I-d):

8. A method of imaging body tissue in a patient, comprising:

administering to the patient an effective amount of one or more compounds according to claim 1 in a pharmaceutically acceptable carrier, and

subjecting the patient to a magnetic resonance imaging procedure.

9. A compound of general formula (III):

in which R 5 is a hydrogen atom or a methyl group, and LG represents an activating leaving group selected from the group consisting of pentafluorophenol, hydroxybenzotriazole, and 3H-[1,2,3]triazolo[4,5-b]pyridine-3-ol.

10. The compound of claim 1 , wherein the compound is:

Tetragadolinium [4,10-bis(carboxylatomethyl)-7-{3,6,12,15-tetraoxo-16-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({2-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}methyl)-4,7,11,14-tetraazaheptadecan-2-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate, or

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

11. A compound of general formula (II), comprising:

in which:

represents a group selected from:

in which * on the A group indicates a point of attachment of the A group with R 1 ;

R 1 represents, independently from each other, a hydrogen atom or a substituent group selected from:

R 3 ,

in which * on the substituent group indicates a point of attachment of the substituent group with A group, with the proviso that zero or only one of the R 1 groups present in the compound represent a hydrogen atom;

n represents an integer of 3 or 4;

R 2 represents, independently from each other, a hydrogen atom or a methyl group;

R 3 represents a group selected from:

in which * on the R 3 group indicates a point of attachment of the R 3 group with a nitrogen on the A group or the substituent group;

R 4 represents, independently from each other, a hydrogen atom or a methyl group; and

R 5 represents, independently from each other, a hydrogen atom or a methyl group;

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

12. The compound of claim 11 , wherein the compound is selected from the group consisting of:

[4,10-bis(carboxylatomethyl)-7-{3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({2-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}methyl)-4,7,11,14-tetraazaheptadecan-2-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate;

{4,10-bis(carboxylatomethyl)-7-[(2R,16R)-3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({(2R)-2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate;

{4,10-bis(carboxylatomethyl)-7-[(2S,16S)-3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({(2S)-2-[4,7,10-tris-(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}-methyl)-4,7,11,14-tetraazaheptadecan-2-yl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate;

2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″,2″″″″″″,2′″″″″″″,2″″″″″″″, 2′″″″″″″″,2″″″″″″″″,2′″″″″″″″″-(1,4,7-triazonane-1,4,7-triyltris{carbonyl-1,4-diazepane-6,1,4-triylbis[(2-oxoethane-2,1-diyl)imino(1-oxopropane-1,2-diyl)-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]})octadecaacetate;

2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″-{1,4,7,10-tetraazacyclododecane-1,4,7,10-tetrayltetrakis[(2-oxoethane-2,1-diyl)imino(1-oxopropane-1,2-diyl)-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]}dodecaacetate;

2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″,2″″″″″″,2′″″″″″″,2″″″″″″″, 2′″″″″″″″,2″″″″″″″″,2′″″″″″″″″-{3,7,10-triazatricyclo[3.3.3.0 1,5 ]undecane-3,7,10-triyltris[carbonyl-(3,6,11,14-tetraoxo-4,7,10,13-tetraazahexadecane-8,2,15-triyl)di-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]}octadecaacetate;

2,2′,2″,2′″,2″″,2′″″,2″″″,2′″″″,2″″″″,2′″″″″,2″″″″″,2′″″″″″-(3,7,9-triazabicyclo[3.3.1]nonane- 3,7-diylbis{carbonyl-1,4-diazepane-6,1,4-triylbis[(2-oxoethane-2,1-diyl)-1,4,7,10-tetraazacyclododecane-10,1,4,7-tetrayl]})dodecaacetate;

{4,10-bis(carboxylatomethyl)-7-[2-oxo-2-({3-({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)-2,2-bis[({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)methyl]propyl}amino)ethyl]-1,4,7,10-tetraazacyclododecan-1-yl}acetate; and

[4,10-bis(carboxylatomethyl)-7-{2,5,11,14-tetraoxo-15-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-8,8-bis({[({[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]acetyl}amino)acetyl]amino}methyl)-3,6,10,13-tetraazapentadec-1-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate,

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

13. The compound of claim 1 , wherein the compound is:

[4,10-bis(carboxylatomethyl)-7-{3,6,12,15-tetraoxo-16-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]-9,9-bis({[({2-[4,7,10-tris(carboxylatomethyl)-1,4,7,10-tetraazacyclododecan-1-yl]propanoyl}amino)acetyl]amino}methyl)-4,7,11,14-tetraazaheptadecan-2-yl}-1,4,7,10-tetraazacyclododecan-1-yl]acetate, or

or a stereoisomer, a tautomer, an N-oxide, a hydrate, a solvate, or a salt thereof, or a mixture of same.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 27, 2019
From: BERGER, MARKUS; LOHRKE, JESSICA; HILGER, CHRISTOPH-STEPHAN; JOST, GREGOR; FRENZEL, THOMAS; SUELZLE, DETLEV; PLATZEK, JOHANNES; PANKNIN, OLAF; PIETSCH, HUBERTUS
To: BAYER PHARMA AKTIENGESELLSCHAFT
Reel/Frame 048450/0181 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 15, 2018
From: BERGER, MARKUS; LOHRKE, JESSICA; HILGER, CHRISTOPH-STEPHAN; JOST, GREGOR; FRENZEL, THOMAS; SUELZLE, DETLEV; PLATZEK, JOHANNES; PANKNIN, OLAF; PIETSCH, HUBERTUS
To: BAYER PHARMA AKTIENGESELLSCHAFT
Reel/Frame 045803/0554 →
Priority Claims (1)
EP 15170658 · Jun 4, 2015 · regional
Continuity (1)
Related Publication 20180169274A1 · Jun 21, 2018
Cited By (1)
US 12,478,696