IP Library Granted Patent US 9,968,612
Granted Patent B2
US 9,968,612 · App. 15/046,213 · Granted May 15, 2018

Method of synthesizing thyroid hormone analogs and polymorphs thereof

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Quick Facts
Patent No.
US 9,968,612
App. No.
15/046,213
Granted
May 15, 2018
Kind
B2
Abstract

The disclosure describes methods of synthesis of pyridazinone compounds as thyroid hormone analogs and their prodrugs. Preferred methods according to the disclosure allow for large-scale preparation of pyridazinone compounds having high purity. In some embodiments, preferred methods according to the disclosure also allow for the preparation of pyridazinone compounds in better yield than previously used methods for preparing such compounds. Also disclosed are morphic forms of a pyridazinone compound. Further disclosed is a method for treating resistance to thyroid hormone in a subject having at least one TRβ mutation.

Claims (21)

1. A method for treating a resistance to thyroid hormone (RTH) syndrome in a subject having at least one TRβ mutation and a disease or disorder selected from the group consisting of fatty liver disease, attention deficit hyperactivity disorder, a learning disability, thyroid axis alteration, atherosclerosis, a cardiovascular disorder, tachycardia, hyperkinetic behavior, hypothyroidism, goiter, hearing loss, delayed bone age, and thyroid cancer, comprising administering to the subject a therapeutically effective amount of 2-(3,5-dichloro-4-((5-isopropyl-6-oxo-1,6-dihydropyridazin-3-yl)oxy)pheny-1)-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile (“Compound A”).

2. The method of claim 1 , wherein said disease or disorder is selected from the group consisting of fatty liver disease, attention deficit hyperactivity disorder, a learning disability, atherosclerosis, and a cardiovascular disorder.

3. The method of claim 1 , wherein said TRβ mutation is selected from the group consisting of a substitution of threonine (T) for the wild type residue alanine (A) at amino acid position 234 of SEQ ID NO: 1 (A234T); a substitution of glutamine (Q) for the wild type residue arginine (R) at amino acid position 243 of SEQ ID NO: 1 (R243Q); a substitution of histidine (H) for the wild type residue arginine (R) at amino acid position 316 of SEQ ID NO: 1 (R316H); and a substitution of threonine (T) for the wild type residue alanine (A) at amino acid position 317 of SEQ ID NO: 1 (A317T).

4. The method of claim 1 , wherein Compound A comprises a morphic form (Form I) characterized by an X-ray powder diffraction pattern including peaks at about 10.5, 18.7, 22.9, 23.6, and 24.7 degrees 2θ.

5. The method of claim 4 , wherein the morphic form is characterized by an X-ray powder diffraction pattern further including peaks at about 8.2, 11.2, 15.7 16.4, 17.7, 30.0, and 32.2 degrees 2θ.

6. The method of claim 4 , wherein the morphic form is characterized by an X-ray powder diffraction pattern substantially similar to that set forth in FIG. 1 .

7. The method of claim 4 , wherein the morphic form has a purity of 95% or greater.

8. The method of claim 2 , wherein Compound A comprises a morphic form (Form I) characterized by an X-ray powder diffraction pattern including peaks at about 10.5, 18.7, 22.9, 23.6, and 24.7 degrees 2θ.

9. The method of claim 8 , wherein the morphic form is characterized by an X-ray powder diffraction pattern further including peaks at about 8.2, 11.2, 15.7 16.4, 17.7, 30.0, and 32.2 degrees 2θ.

10. The method of claim 8 , wherein the morphic form is characterized by an X-ray powder diffraction pattern substantially similar to that set forth in FIG. 1 .

11. The method of claim 8 , wherein the morphic form has a purity of 95% or greater.

12. The method of claim 3 , wherein Compound A comprises a morphic form (Form I) characterized by an X-ray powder diffraction pattern including peaks at about 10.5, 18.7, 22.9, 23.6, and 24.7 degrees 2θ.

13. The method of claim 12 , wherein the morphic form is characterized by an X-ray powder diffraction pattern further including peaks at about 8.2, 11.2, 15.7 16.4, 17.7, 30.0, and 32.2 degrees 2θ.

14. The method of claim 12 , wherein the morphic form is characterized by an X-ray powder diffraction pattern substantially similar to that set forth in FIG. 1 .

15. The method of claim 12 , wherein the morphic form has a purity of 95% or greater.

16. A method for treating a resistance to thyroid hormone (RTH) syndrome in a subject having at least one TRβ mutation and a disease or disorder selected from the group consisting of fatty liver disease, attention deficit hyperactivity disorder, a learning disability, thyroid axis alteration, atherosclerosis, a cardiovascular disorder, tachycardia, hyperkinetic behavior, hypothyroidism, goiter, hearing loss, delayed bone age, and thyroid cancer, comprising administering to the subject a therapeutically effective amount of a compound of Formula (IV):

wherein

R 3 is H or CH 2 R a , in which R a is hydroxyl, O-linked amino acid, −OP(O)(OH) 2 or OC(O)—R b , R b being lower alkyl, alkoxy, alkyl acid, or cycloalkyl; and

R 4 and R 5 together are —N═C(R c )—C(O)—NH—C(O)—, a in which R c is H or cyano.

17. The method of claim 16 , wherein said disease or disorder is selected from the group consisting of fatty liver disease, attention deficit hyperactivity disorder, a learning disability, atherosclerosis, and a cardiovascular disorder.

18. The method of claim 16 , wherein said TRβ mutation is selected from the group consisting of a substitution of threonine (T) for the wild type residue alanine (A) at amino acid position 234 of SEQ ID NO: 1 (A234T); a substitution of glutamine (Q) for the wild type residue arginine (R) at amino acid position 243 of SEQ ID NO: 1 (R243Q); a substitution of histidine (H) for the wild type residue arginine (R) at amino acid position 316 of SEQ ID NO: 1 (R316H); and a substitution of threonine (T) for the wild type residue alanine (A) at amino acid position 317 of SEQ ID NO: 1 (A317T).

Assignments (3)
SECURITY INTEREST Recorded Jul 17, 2025
From: MADRIGAL PHARMACEUTICALS, INC.
To: LSI FINANCING LLC, AS ADMINISTRATIVE AGENT
Reel/Frame 072038/0693 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2020
From: CHOI, DUK SOON; SHU, LIANHE; WANG, PING
To: HOFFMANN-LA ROCHE INC.
Reel/Frame 053008/0346 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 21, 2016
From: TAUB, REBECCA; REYNOLDS, CHARLES H.
To: MADRIGAL PHARMACEUTICALS, INC.
Reel/Frame 038339/0893 →