IP Library Granted Patent US 8,748,455
Granted Patent B2
US 8,748,455 · App. 13/817,124 · Granted Jun 10, 2014

Solid forms of a pharmaceutically active substance

Inventors: Prabha N. Ibrahim (Mountain View, CA); Gary Conard Visor (Castro Valley, CA); Shan-Ming Kuang (Florence, SC); Baoshu Zhao (Florence, SC); Ralph Diodone (Breisach, DE); Karsten Fähnrich (Grenzach-Wyhlen, DE); Urs Schwitter (Reinach, CH)
Assignees: Plexxikon Inc.; Hoffman-La Roche Inc.
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Quick Facts
Patent No.
US 8,748,455
App. No.
13/817,124
Granted
Jun 10, 2014
Kind
B2
Abstract

The present invention provides solid forms of the compound of formula 1 and pharmaceutical uses thereof.

Claims (42)

1. A solid form of the compound of formula 1,

wherein said solid form is selected from the group consisting of

a) a substantially amorphous form of compound 1 selected from form XVII, XVIII, XIX, XX, XXI, XXII, XXIII, XXIV, XXV, XXVI or combinations thereof, wherein the compound 1 is molecularly dispersed;

b) a solvate selected from form III, IV, V, VI, VII, IX, X, XI, XII, XIII, XIV or XV;

c) a polymorph selected from form VIII or XVI; and

d) the sulfuric acid-, hydrobromic acid- or hydrochloric acid salt of compound 1.

2. The solid form of claim 1 , selected from a substantially amorphous form of compound 1 selected from form XVII, XVIII, XIX, XX, XXI, XXII, XXIII, XXIV, XXV, XXVI or combinations thereof, wherein compound 1 is molecularly dispersed within a polymer matrix.

3. The solid form (XVII) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 20 .

4. The solid form (XVIII) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 21 .

5. The solid form (XIX) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 22 .

6. The solid form (XX) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 23 .

7. The solid form (XXI) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 24 .

8. The solid form (XXII) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 25 .

9. The solid form (XXIII) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 26 .

10. The solid form (XXIV) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 27 .

11. The solid form (XXV) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 28 .

12. The solid form (XXVI) of claim 2 , characterized by an X-ray powder diffraction pattern substantially as shown in FIG. 29 .

13. The solid form claim 2 , wherein the solid form is prepared by a spray dispersion process.

14. The solid form of claim 2 , wherein the polymer is selected from hydroxypropyl methyl cellulose acetate succinate (HPMCAS), hydroxypropylmethyl cellulose, methacrylic acid copolymers, polyvinylpyrrolidone (povidone), 4-vinylpyrrolidone-vinyl acetate copolymer (copovidone) or copolymers of methacrylic acid and ethylacrylate (EUDRAGIT® L100-55).

15. A pharmaceutical composition comprising at least one solid form according to claim 2 , or a pharmaceutically acceptable salt thereof, and a pharmaceutically acceptable carrier, additives or excipients.

16. The solid form of claim 1 , selected from a solvate of form III, IV, V, VI, VII, IX, X, XI, XII, XIII, XIV or XV.

17. The solid form of claim 1 , selected from a polymorph of form VIII or XVI.

18. The solid form of claim 1 , selected from the sulfuric acid-, hydrobromic acid- or hydrochloric acid salt of compound 1.

19. A solid form (form III) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 9.5, 10.0, 13.0, 16.7, 18.7, 20.1, 21.0 and 25.6 degrees 2Theta (±0.2 degrees 2Theta).

20. A solid form (form IV) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 5.5, 7.4, 11.0, 13.4, 14.8, 16.0, 16.7, 17.1, 17.9, 19.1, 19.5, 20.1, 20.5, 20.9, 21.2, 22.2, 23.0, 23.6, 24.2, 24.5 and 25.1 degrees 2Theta (±0.2 degrees 2Theta).

21. A solid form (form V) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 12.7, 13.1, 14.3, 16.3, 19.0, 20.1, 22.4, 25.1, 27.1 and 28.9 degrees 2Theta (±0.2 degrees 2Theta).

22. A solid form (form VI) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 7.8, 10.3, 11.4, 11.8, 15.1, 15.6, 16.1, 16.6, 18.6, 18.9, 19.2, 20.4, 21.0, 21.6, 22.8, 24.6, 25.1, 25.8, 26.1, 27.4 and 28.8 degrees 2Theta (±0.2 degrees 2Theta).

23. A solid form (form VII) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 7.6, 9.4, 9.9, 13.1, 15.9, 16.2, 17.0, 18.1, 18.8, 19.9, 20.5, 20.7, 21.4, 21.8, 24.3, 24.9 and 25.3 degrees 2Theta (±0.2 degrees 2Theta).

24. A solid form (form IX) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 9.5, 9.9, 13.0, 15.9, 16.4, 17.0, 17.9, 18.7, 19.9, 20.7, 21.7, 24.8 and 25.1 degrees 2Theta (±0.2 degrees 2Theta).

25. A solid form (form X) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 7.4, 9.2, 10.8, 13.6, 14.9, 19.0, 20.2, 21.4, 22.4, 23.7, 25.5, 27.0 and 29.8 degrees 2Theta (±0.2 degrees 2Theta).

26. A solid form (form XI) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 8.0, 12.1, 12.6, 13.4, 13.9, 14.8, 16.2, 17.6, 18.5, 19.2, 20.1, 21.0, 21.4, 21.7, 23.5, 25.3, 25.5, 26.6, 27.0 and 30.8 degrees 2Theta (±0.2 degrees 2Theta).

27. A solid form (form XII) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 7.5, 9.9, 12.1, 13.6, 16.2, 16.7, 17.1, 17.5, 18.3, 18.5, 20.1, 21.7, 22.4, 23.4, 24.3, 25.6, 26.9 and 31.6 degrees 2Theta (±0.2 degrees 2Theta).

28. A solid form (form XIII) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 5.1, 5.8, 6.9, 15.3, 16.2, 17.4, 18.4, 18.9, 19.5, 20.4, 21.1, 21.5, 22.2, 22.6, 25.2 and 25.7 degrees 2Theta (±0.2 degrees 2Theta).

29. A solid form (form XIV) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 5.2, 10.2, 12.9, 13.9, 17.1, 17.6, 18.7, 19.8, 20.1, 20.5, 21.0, 21.7, 22.8, 24.1, 25.1, 25.5, 27.1 and 27.4 degrees 2Theta (±0.2 degrees 2Theta).

30. A solid form (form XV) according to claim 16 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 12.6, 13.8, 14.6, 16.2, 16.6, 17.8, 18.3, 20.4, 20.7, 21.4, 22.4, 23.2, 24.2, 24.5, 25.5, 26.9, 27.8 and 28.7 degrees 2Theta (±0.2 degrees 2Theta).

31. A solid form designated “pattern 6” according to claim 16 , characterized in that it comprises signals in its X-ray powder diffraction curve at positions 7.0, 8.4, 8.9, 13.0, 13.8, 17.7, 18.8, 20.7, 25.8 and 29.7 degrees 2Theta (±0.2 degrees 2Theta).

32. A solid form (form VIII) according to claim 17 , characterized in that it comprises signals in its X-ray powder diffraction curve at positions 5.0, 11.3, 11.6, 12.0, 13.8, 16.2, 16.7, 19.0, 20.1, 20.8, 22.5 and 27.1 degrees 2Theta (±0.2 degrees 2Theta).

33. A solid form (form XVI) according to claim 17 , characterized by its Raman spectrum as presented in FIG. 15 .

34. The sulfuric acid salt according to claim 18 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 4.7, 6.7, 10.6, 13.3, 14.5, 15.7, 16.4, 18.3, 18.6, 18.9, 19.5, 20.1, 20.9, 21.2, 23.2, 23.7, 24.0, 26.9 and 30.0 degrees 2Theta (±0.2 degrees 2Theta).

35. The hydrobromic acid salt according to claim 18 , characterized by an X-ray powder diffraction pattern comprising characteristic peas at approximately 5.7, 6.8, 11.4, 13.6, 18.1, 19.8, 20.2, 21.4, 21.8, 24.6, 26.1, 27.3 and 29.2 degrees 2Theta (±0.2 degrees 2Theta).

36. The hydrochloric acid salt according to claim 18 , characterized by an X-ray powder diffraction pattern comprising characteristic peaks at approximately 6.6, 7.8, 11.2, 12.6, 14.1, 14.7, 16.3, 17.8, 19.3, 19.6, 20.7, 21.5, 22.7, 24.1, 25.4 and 25.8 degrees 2Theta (±0.2 degrees 2Theta).

37. A pharmaceutical composition comprising at least one of the solid forms according to claim 16 , together with pharmaceutically acceptable additives, carriers or excipients.

Assignments (13)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 24, 2013
From: IBRAHIM, PRABHA N.; VISOR, GARY C.
To: PLEXXIKON INC.
Reel/Frame 031472/0207 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 24, 2013
From: ZHAO, BAOSHU
To: HOFFMAN-LA ROCHE INC.
Reel/Frame 031472/0312 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 24, 2013
From: KUANG, SHAN-MING
To: HOFFMAN-LA ROCHE INC.
Reel/Frame 031472/0354 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 24, 2013
From: DIODONE, RALPH; F?HNRICH, KARSTEN; SCHWITTER, URS
To: F. HOFFMAN-LA ROCHE AG
Reel/Frame 031472/0645 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 24, 2013
From: F. HOFFMAN-LA ROCHE AG
To: HOFFMAN-LA ROCHE INC.
Reel/Frame 031472/0672 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 2, 2013
From: F. HOFFMANN-LA ROCHE AG
To: HOFFMANN-LA ROCHE INC.
Reel/Frame 030333/0825 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 2, 2013
From: HOFFMANN-LA ROCHE INC.
To: ROCHE CAROLINA INC.
Reel/Frame 030333/0755 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 26, 2013
From: DIODONE, RALPH; FAEHNRICH, KARSTEN
To: F. HOFFMANN-LA ROCHE AG
Reel/Frame 030084/0772 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 26, 2013
From: F. HOFFMANN-LA ROCHE AG
To: HOFFMANN-LA ROCHE INC.
Reel/Frame 030084/0789 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 26, 2013
From: HOFFMANN-LA ROCHE INC.
To: F. HOFFMANN-LA ROCHE AG
Reel/Frame 030084/0853 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 26, 2013
From: DIODONE, RALPH; FAEHNRICH, KARSTEN; SCHWITTER, URS
To: F. HOFFMANN-LA ROCHE AG
Reel/Frame 030085/0746 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 26, 2013
From: ZHAO, BAOSHU
To: HOFFMANN-LA ROCHE INC.
Reel/Frame 030084/0617 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 26, 2013
From: KUANG, SHAN-MING
To: HOFFMANN-LA ROCHE INC.
Reel/Frame 030084/0658 →
Continuity (2)
Provisional Application 61444866 · Feb 21, 2011
Related Publication 20140039002A1 · Feb 6, 2014