IP Library Granted Patent US 9,707,211
Granted Patent B2
US 9,707,211 · App. 15/015,403 · Granted Jul 18, 2017

Trifluoromethyl pyrazolyl guanidine F

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Quick Facts
Patent No.
US 9,707,211
App. No.
15/015,403
Granted
Jul 18, 2017
Kind
B2
Abstract

The invention provides trifluoromethyl pyrazolyl guanidine compounds that inhibit F 1 F 0 -ATPase, and methods of using trifluoromethyl pyrazolyl guanidine compounds as therapeutic agents to treat medical disorders, such as an immune disorder, inflammatory condition, or cancer.

Claims (248)

1. An oral formulation selected from an enteric-coated tablet and an enteric-coated capsule, wherein the oral formulation comprises a pharmaceutically acceptable carrier and a compound represented by Formula I:

or a geometric isomer or tautomer; or a pharmaceutically acceptable salt of any of the foregoing; wherein R 1 is a chloro group located at either the meta-position or para-position of the phenyl group to which it is attached.

2. The oral formulation of claim 1 , wherein the compound is represented by:

or a geometric isomer or tautomer; or a pharmaceutically acceptable salt of any of the foregoing.

3. The oral formulation of claim 1 , wherein the compound is represented by:

or a geometric isomer or tautomer.

4. The oral formulation of claim 1 , wherein the compound is represented by:

5. The oral formulation of claim 1 , wherein the compound is crystalline compound 3-chloro-N-(((3-chloro-5-fluorophenyl)amino)((5-(trifluoromethyl)-1H-pyrazol-3-yl)amino)methylene)benzamide.

6. The oral formulation of claim 5 , wherein the crystalline compound exhibits an X-ray powder diffraction pattern comprising peaks at the following diffraction angles (2θ): 6.2±0.2, 7.1±0.2, 9.4±0.2, 10.7±0.2, 15.6±0.2, 19.0±0.2, 20.0±0.2, and 25.2±0.2.

7. The oral formulation of claim 6 , wherein for the X-ray powder diffraction pattern the relative intensity of the peak at said diffraction angles (2θ) is at least 30%.

8. The oral formulation of claim 6 , wherein the crystalline compound is characterized by the following X-ray powder diffraction pattern expressed in terms of diffraction angle 2θ, inter-planar distances d, and relative intensity (expressed as a percentage with respect to the most intense peak):

Relative

Angle [2θ]

d-spacing [Å]

Intensity [%]

6.2

14.3

53.8

7.1

12.4

69.6

9.4

9.4

53.8

10.7

8.3

51.0

12.9

6.9

34.6

15.6

5.7

92.8

16.4

5.4

29.1

17.9

4.9

44.0

19.0

4.7

100.0

20.0

4.4

62.6

21.9

4.1

38.9

23.6

3.8

51.4

25.2

3.5

57.8

27.3

3.3

24.0

28.4

3.1

15.8

35.0

2.6

10.0.

9. The oral formulation of claim 5 , wherein the crystalline composed exhibits an X-ray powder diffraction pattern comprising peaks at the following diffraction angles (2θ): 6.3±0.2, 7.3±0.2, 11.0±0.2, 12.8±0.2, 16.9±0.2, 19.2±0.2, 20.6±0.2, 22.2±0.2, 25.7±0.2, 26.0±0.2, and 35.7±0.2.

10. The oral formulation of claim 9 , wherein the relative intensity of the peak at said diffraction angles (2θ) is at least 15%.

11. The oral formulation of claim 9 , wherein the crystalline compound is characterized by the following X-ray powder diffraction pattern expressed in terms of diffraction angle 2θ, inter-planar distances d, and relative intensity (expressed as a percentage with respect to the most intense peak):

Relative

Angle [2θ]

d-spacing [Å]

Intensity [%]

6.33

13.95

65.8

7.32

12.06

100.0

9.73

9.08

14.8

11.03

8.01

55.9

12.76

6.93

18.3

13.27

6.67

9.7

14.75

6.00

9.3

16.07

5.51

12.7

16.91

5.24

27.2

18.45

4.80

9.9

19.18

4.62

42.0

19.53

4.54

8.3

20.56

4.31

19.8

22.20

4.00

88.4

22.51

3.95

43.5

23.11

3.85

56.1

23.55

3.77

29.0

25.65

3.47

48.8

25.96

3.43

100.0

26.75

3.33

26.2

28.03

3.18

52.6

29.03

3.07

44.7

29.51

3.02

29.3

30.45

2.93

20.0

31.49

2.84

17.8

31.82

2.81

20.4

32.27

2.77

29.9

33.15

2.70

16.8

34.18

2.62

12.9

35.66

2.52

59.6

36.03

2.49

17.7

36.84

2.44

13.5

37.75

2.38

14.8

38.27

2.35

10.9

38.99

2.31

13.6

39.71

2.27

13.5

42.15

2.14

11.2

43.46

2.08

13.7

44.19

2.05

8.3

44.55

2.03

13.1

45.96

1.97

16.3

46.46

1.95

16.6

48.33

1.88

9.4

49.33

1.85

9.9

50.27

1.81

9.3

50.48

1.81

9.9

51.25

1.78

8.2

51.45

1.77

9.5

53.86

1.70

9.1

55.63

1.65

9.8

56.54

1.63

6.5

57.53

1.60

8.8

59.28

1.56

6.4.

12. The oral formulation of claim 9 , wherein the X-ray powder diffraction pattern is substantially as shown in FIG. 5 .

13. The oral formulation of claim 10 , wherein the crystalline compound has a melting point onset as determined by differential scanning calorimetry in the range of from about 158 degrees Celsius to about 165 degrees Celsius.

14. The oral formulation of claim 10 , wherein the crystalline compound has a differential scanning calorimetry curve substantially the same as shown in FIG. 6 .

15. The oral formulation of claim 2 , wherein the oral formulation is an enteric-coated tablet.

16. The oral formulation of claim 9 , wherein the oral formulation is an enteric-coated tablet.

17. The oral formulation of claim 2 , wherein the oral formulation is an enteric-coated capsule.

18. The oral formulation of claim 9 , wherein the oral formulation is an enteric-coated capsule.

19. A method of treating a disorder selected from the group consisting of an immune disorder and inflammatory disorder, comprising orally administering to a human patient in need thereof a therapeutically effective amount of an oral formulation of claim 2 in order to ameliorate a symptom of the disorder.

20. The method of claim 19 , wherein the disorder is inflammatory bowel disease.

21. The method of claim 19 , wherein the disorder is ulcerative colitis.

22. The method of claim 19 , wherein the disorder is Crohn's disease.

23. The method of claim 19 , wherein the oral formulation is an oral formulation of claim 2 .

24. The method of claim 20 , wherein the oral formulation is an oral formulation of claim 2 .

25. The method of claim 20 , wherein the oral formulation is an oral formulation of claim 9 .

26. The method of claim 21 , wherein the oral formulation is an oral formulation of claim 2 .

27. The method of claim 21 , wherein the oral formulation is an oral formulation of claim 9 .

28. The method of claim 21 , wherein the oral formulation is an oral formulation of claim 15 .

29. The method of claim 21 , wherein the oral formulation is an oral formulation of claim 16 .

30. The method of claim 22 , wherein the oral formulation is an oral formulation of claim 2 .

Assignments (4)
SECURITY INTEREST Recorded Jan 3, 2019
From: LYCERA CORP.
To: WILMINGTON TRUST, NATIONAL ASSOCIATION
Reel/Frame 048002/0201 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 2, 2017
From: WANG, JIAN; ZHOU, PENG
To: CRYSTAL PHARMATECH
Reel/Frame 042576/0016 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 2, 2017
From: HURD, ALEXANDER R.; TAYLOR, CLARKE B.
To: LYCERA CORPORATION
Reel/Frame 042576/0038 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 2, 2017
From: CRYSTAL PHARMATECH
To: LYCERA CORPORATION
Reel/Frame 042576/0045 →