IP Library Granted Patent US 11,161,802
Granted Patent B2
US 11,161,802 · App. 16/778,696 · Granted Nov 2, 2021

L-ornithine phenyl acetate and methods of making thereof

Inventors: Keith Anderson (San Diego, CA); Jim Behling (Eagle River, WI); Christine Henderson Dougan (Glasgow, GB); Stephen William Watt (Tranent, GB); Peter Manini (Giubiasco, CH); Attilia Figini (Mendrisio, CH)
Assignee: Ocera Therapeutics, Inc.
C07C227/40A61K31/192A61K31/198A61K31/205C07C51/42C07C57/32C07C227/42C07C229/26
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Quick Facts
Patent No.
US 11,161,802
App. No.
16/778,696
Granted
Nov 2, 2021
Kind
B2
Abstract

Disclosed herein are forms of L-ornithine phenyl acetate and methods of making the same. A crystalline form may, in some embodiments, be Forms I, II, III and V, or mixtures thereof. The crystalline forms may be formulated for treating subjects with liver disorders, such as hepatic encephalopathy. Accordingly, some embodiments include formulations and methods of administering L-ornithine phenyl acetate.

Claims (17)

1. A process for preparing L-ornithine phenylacetate, comprising

intermixing phenylacetic acid or a salt thereof with an L-ornithine acetate solution to form a reaction mixture; and

isolating a composition comprising a crystalline form of L-ornithine phenylacetate from the reaction mixture.

2. The process of claim 1 , wherein the L-ornithine acetate solution is prepared by intermixing an L-ornithine salt with acetic acid in a first solvent.

3. The process of claim 2 , wherein the L-ornithine salt is L-ornithine halide salt.

4. The process of claim 3 , wherein the L-ornithine salt is L-ornithine hydrochloride.

5. The process of claim 2 , wherein the molar ratio of the L-ornithine salt to acetic acid is at least 1:2.

6. The process of claim 2 , wherein the first solvent comprises water.

7. The process of claim 1 , further comprising adding a second solvent to the reaction mixture before isolating the crystalline form of L-ornithine phenylacetate.

8. The process of claim 7 , wherein the second solvent comprises isopropyl alcohol (IPA).

9. The process of claim 1 , further comprising recrystallizing the isolated crystalline form of L-ornithine phenylacetate.

10. The process of claim 1 , wherein the crystalline form of L-ornithine phenylacetate exhibits an X-ray powder diffraction pattern comprising at least three characteristic peaks, wherein said characteristic peaks are selected from the group consisting of peaks at approximately 6.0°, 13.9°, 14.8°, 17.1°, 17.8° and 24.1° 2θ.

11. The process of claim 10 , wherein the crystalline form of L-ornithine phenylacetate exhibits an X-ray powder diffraction pattern comprising characteristic peaks selected from the group consisting of peaks at approximately 6.0°, 13.9°, 14.8°, 17.1°, 17.8° and 24.1° 2θ.

12. The process of claim 1 , wherein the crystalline form of L-ornithine phenylacetate exhibits an X-ray powder diffraction pattern comprising at least three characteristic peaks, wherein said characteristic peaks are selected from the group consisting of peaks at approximately 4.9°, 13.2°, 17.4°, 20.8° and 24.4° 2θ.

13. The process of claim 12 , wherein the crystalline form of L-ornithine phenylacetate exhibits an X-ray powder diffraction pattern comprising characteristic peaks selected from the group consisting of peaks at approximately 4.9°, 13.2°, 17.4°, 20.8° and 24.4° 2θ.

14. The process of claim 1 , wherein the crystalline form of L-ornithine phenylacetate exhibits an X-ray powder diffraction pattern comprising at least three characteristic peaks, wherein said characteristic peaks are selected from the group consisting of peaks at approximately 5.8°, 14.1°, 18.6°, 19.4°, 22.3° and 24.8° 2θ.

15. The process of claim 14 , wherein the crystalline form of L-ornithine phenylacetate exhibits an X-ray powder diffraction pattern comprising characteristic peaks selected from the group consisting of peaks at approximately 5.8°, 14.1°, 18.6°, 19.4°, 22.3° and 24.8° 2θ.

Assignments (18)
RELEASE OF SECURITY INTEREST Recorded Aug 14, 2025
From: ACQUIOM AGENCY SERVICES LLC
To: MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY; MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; OCERA THERAPEUTICS LLC; SPECGX LLC; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC
Reel/Frame 072324/0740 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 25, 2024
From: OCERA THERAPEUTICS LLC
To: AMALIVE LIMITED
Reel/Frame 069017/0200 →
RELEASE OF SECURITY INTEREST Recorded Oct 7, 2024
From: ACQUIOM AGENCY SERVICES LLC
To: MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; SPECGX LLC; OCERA THERAPEUTICS, INC.; STRATATECH CORPORATION; VTESSE LLC; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY; MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; SUCAMPO PHARMA AMERICAS LLC
Reel/Frame 068810/0460 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 31, 2024
From: OCERA THERAPEUTICS, INC.
To: OCERA THERAPEUTICS LLC
Reel/Frame 066403/0804 →
RELEASE OF SECURITY INTEREST Recorded Nov 30, 2023
From: WILMINGTON SAVINGS FUND SOCIETY, FSB, AS SECOND LIEN COLLATERAL AGENT
To: OCERA THERAPEUTICS LLC (F/K/A OCERA THERAPEUTICS, INC.); MALLINCKRODT HOSPITAL PRODUCTS IP UNLIMITED COMPANY (F/K/A MALLINCKRODT HOSPITAL PRODUCTS IP LIMITED); STRATATECH CORPORATION
Reel/Frame 065712/0988 →
RELEASE OF PATENT SECURITY INTERESTS RECORDED AT REEL 060434, FRAME 0536 Recorded Nov 16, 2023
From: DEUTSCHE BANK AG NEW YORK BRANCH, AS COLLATERAL AGENT
To: MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; SPECGX LLC; OCERA THERAPEUTICS, INC.; STRATATECH CORPORATION; VTESSE LLC; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY; MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; SUCAMPO PHARMA AMERICAS LLC
Reel/Frame 065601/0347 →
RELEASE OF PATENT SECURITY INTERESTS RECORDED AT REEL 052456, FRAME 0158 Recorded Nov 16, 2023
From: DEUTSCHE BANK AG NEW YORK BRANCH, AS COLLATERAL AGENT
To: MALLINCKRODT INTERNATIONAL FINANCE S.A.; MALLINCKRODT CB LLC; MALLINCKRODT FINANCE GMBH; MALLINCKRODT US HOLDINGS LLC (F/K/A MALLINCKRODT US HOLDINGS INC.); MALLINCKRODT CARRIBEAN, INC.; MALLINCKRODT US POOL LLC; MNK 2011 LLC (F/K/A MALLINCKRODT INC.); LUDLOW LLC (F/K/A LUDLOW CORPORATION); CNS THERAPEUTICS, INC.; MALLINCKRODT ENTERPRISES HOLDINGS LLC (F/K/A MALLINCKRODT ENTERPRISES HOLDINGS, INC.); MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; LAFAYETTE PHARMACEUTICALS LLC; LIEBEL-FLARSHEIM COMPANY LLC; MALLINCKRODT BRAND PHARMACEUTICALS LLC (F/K/A MALLINCKRODT BRAND PHARMACEUTICALS, INC.); MALLINCKRODT VETERINARY, INC.; MALLINCKRODT US HOLDINGS LLC; IMC EXPLORATION COMPANY; MEH, INC.; MALLINCKRODT HOSPITAL PRODUCTS IP UNLIMITED COMPANY (F/K/A MALLINCKRODT HOSPITAL PRODUCTS IP LIMITED); MALLINCKRODT ARD IP UNLIMITED COMPANY (F/K/A MALLINCKRODT ARD IP LIMITED); OCERA THERAPEUTICS LLC (F/K/A OCERA THERAPEUTICS, INC.); SPECGX LLC; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC (F/K/A VTESSE INC.); MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY (F/K/A MALLINCKRODT PHARMA IP TRADING D.A.C.); INFACARE PHARMACEUTICAL CORPORATION; ST SHARED SERVICES LLC; THERAKOS, INC.; IKARIA THERAPEUTICS LLC; INO THERAPEUTICS LLC
Reel/Frame 065609/0133 →
RELEASE OF SECURITY INTERESTS IN PATENTS AT REEL 060389/FRAME 0913 Recorded Nov 15, 2023
From: WILMINGTON SAVINGS FUND SOCIETY, FSB, AS SECOND LIEN COLLATERAL AGENT
To: OCERA THERAPEUTICS LLC (F/K/A OCERA THERAPEUTICS, INC.); MALLINCKRODT LLC; MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY; SPECGX LLC; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC; MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED
Reel/Frame 065583/0465 →
SECURITY INTEREST Recorded Nov 15, 2023
From: MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY; MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; OCERA THERAPEUTICS LLC; SPECGX LLC; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC
To: ACQUIOM AGENCY SERVICES LLC
Reel/Frame 065595/0376 →
NOTICE OF GRANT OF SECURITY INTEREST IN INTELLECTUAL PROPERTY Recorded Jun 22, 2022
From: MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; SPECGX LLC; OCERA THERAPEUTICS, INC.; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC; MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED; MALLINCKRODT PHARMA IP TRADING UNLIMITED COMPANY
To: DEUTSCHE BANK AG NEW YORK BRANCH
Reel/Frame 060434/0536 →
SECURITY INTEREST Recorded Jun 17, 2022
From: MALLINCKRODT ENTERPRISES LLC; MALLINCKRODT LLC; SPECGX LLC; OCERA THERAPEUTICS, INC.; STRATATECH CORPORATION; SUCAMPO PHARMA AMERICAS LLC; VTESSE LLC; MALLINCKRODT PHARMACEUTICALS IRELAND LIMITED
To: WILMINGTON SAVINGS FUND SOCIETY, FSB, AS SECOND LIEN COLLATERAL AGENT
Reel/Frame 060389/0913 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 27, 2021
From: MANINI, PETER; FIGINI, ATTILIA
To: HELSINN ADVANCED SYNTHESIS SA
Reel/Frame 057614/0343 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 27, 2021
From: WATT, STEPHEN WILLIAM; DOUGAN, CHRISTINE HENDERSON
To: SOLID FORM SOLUTIONS LTD.
Reel/Frame 057614/0431 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 27, 2021
From: SOLID FORM SOLUTIONS LTD.
To: OCERA THERAPEUTICS, INC.
Reel/Frame 057613/0006 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 27, 2021
From: HELSINN ADVANCED SYNTHESIS SA
To: OCERA THERAPEUTICS, INC.
Reel/Frame 057620/0183 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 27, 2021
From: ANDERSON, KEITH; BEHLING, JIM
To: OCERA THERAPEUTICS, INC.
Reel/Frame 057613/0433 →
SECURITY INTEREST Recorded Apr 22, 2020
From: MALLINCKRODT HOSPITAL PRODUCTS IP LIMITED; OCERA THERAPEUTICS, INC.; ST SHARED SERVICES LLC
To: WILMINGTON SAVINGS FUND SOCIETY, FSB, AS SECOND LIEN COLLATERAL AGENT
Reel/Frame 052463/0396 →
NOTICE OF GRANT OF SECURITY INTEREST IN INTELLECTUAL PROPERTY Recorded Apr 21, 2020
From: MALLINCKRODT HOSPITAL PRODUCTS IP LIMITED
To: DEUTSCHE BANK AG NEW YORK BRANCH, AS COLLATERAL AGENT
Reel/Frame 052456/0158 →