IP Library Granted Patent US 10,829,443
Granted Patent B2
US 10,829,443 · App. 16/331,069 · Granted Nov 10, 2020

Solvate form of (R)-2-amino-3-phenylpropyl carbamate

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Quick Facts
Patent No.
US 10,829,443
App. No.
16/331,069
Granted
Nov 10, 2020
Kind
B2
Abstract

The present invention relates to a newly identified solvate form of (i?)-2-amino-3-phenylpropyl carbamate (APC) hydrochloride, a method of preparing APC hydrochloride, and methods of using the same to treat disorders. The invention further relates to methods of producing APC hydrochloride with increased purity.

Claims (27)

1. A solvate form of (R)-2-amino-3-phenylpropyl carbamate hydrochloride characterized by a powder x-ray diffraction pattern substantially the same as that shown in FIG. 1 Form B.

2. The solvate form of claim 1 , further characterized by differential scanning calorimetry as having a broad endotherm with onset at 69.1° C. and peak at 71.7° C. and a sharp endotherm with onset at 182.5° C. and peak at 183.6° C.

3. The solvate form of claim 1 , wherein the solvate form is a hemihydrate.

4. The solvate form of claim 1 , further characterized as being produced by slurrying (R)-2-amino-3-phenylpropyl carbamate hydrochloride in acetonitrile/water (95%/5% v/v).

5. A process of preparing a solvate form of (R)-2-amino-3-phenylpropyl carbamate hydrochloride, comprising slurrying (R)-2-amino-3-phenylpropyl carbamate hydrochloride in acetonitrile/water (95%/5% v/v) and collecting the solvate by vacuum filtration.

6. The process of claim 5 , wherein the slurrying is performed at about room temperature.

7. The process of claim 5 , wherein the slurrying is performed for at least about 20 hours.

8. A composition comprising (R)-2-amino-3-phenylpropyl carbamate hydrochloride, wherein at least 30% of the (R)-2-amino-3-phenylpropyl carbamate hydrochloride is the solvate form of claim 1 .

9. The composition of claim 8 , wherein the composition is a dosage form.

10. The composition of claim 9 , wherein the composition is an immediate release oral dosage form.

11. The composition of claim 10 , wherein the composition is a tablet or a capsule.

12. A method of treating narcolepsy, cataplexy, excessive daytime sleepiness, drug addiction, sexual dysfunction, fatigue, fibromyalgia, attention deficit/hyperactivity disorder, restless legs syndrome, depression, bipolar disorder, or obesity in a subject in need thereof, or promoting smoking cessation in a subject in need thereof, comprising administering to the subject the composition of claim 8 .

13. A method of preparing (R)-2-amino-3-phenylpropyl carbamate hydrochloride while minimizing contamination with 2-chloropropane, the method comprising crystallizing (R)-2-amino-3-phenylpropyl carbamate in the presence of aqueous HCl, thereby producing crystals of (R)-2-amino-3-phenylpropyl carbamate hydrochloride.

14. The method of claim 13 , wherein the crystallizing is performed at a temperature of about 25° C. to about 30° C.

15. The method of claim 12 , wherein the subject has excessive daytime sleepiness.

16. The method of claim 13 , further comprising drying the crystals of (R)-2-amino-3-phenylpropyl carbamate hydrochloride at a temperature of about 35° C. or less.

17. The method of claim 13 , wherein the amount of 2-chloropropane in the (R)-2-amino-3-phenylpropyl carbamate hydrochloride is less than about 5 ppm.

18. A solvate form of (R)-2-amino-3-phenylpropyl carbamate hydrochloride characterized by a powder x-ray diffraction pattern having peaks at about 7.0, 13.6, 16.2, 17.4, 17.8, 18.5, 21.0, 21.7, 22.7, 23.0, 24.0, and 27.3±0.2 °2θ.

19. The solvate form of claim 18 , further characterized by differential scanning calorimetry as having a broad endotherm with onset at 69.1° C. and peak at 71.7° C. and a sharp endotherm with onset at 182.5° C. and peak at 183.6° C.

20. The solvate form of claim 18 , wherein the solvate form is a hemihydrate.

21. The solvate form of claim 18 , further characterized as being produced by slurrying (R)-2-amino-3-phenylpropyl carbamate hydrochloride in acetonitrile/water (95%/5% v/v).

22. A composition comprising (R)-2-amino-3-phenylpropyl carbamate hydrochloride, wherein at least 30% of the (R)-2-amino-3-phenylpropyl carbamate hydrochloride is the solvate form of claim 18 .

23. The composition of claim 22 , wherein the composition is a dosage form.

24. The composition of claim 23 , wherein the composition is an immediate release oral dosage form.

25. The composition of claim 24 , wherein the composition is a tablet or a capsule.

26. A method of treating narcolepsy, cataplexy, excessive daytime sleepiness, drug addiction, sexual dysfunction, fatigue, fibromyalgia, attention deficit/hyperactivity disorder, restless legs syndrome, depression, bipolar disorder, or obesity in a subject in need thereof, or promoting smoking cessation in a subject in need thereof, comprising administering to the subject the composition of claim 22 .

27. The method of claim 26 , wherein the subject has excessive daytime sleepiness.

Assignments (9)
SECURITY INTEREST Recorded May 9, 2025
From: AXSOME THERAPEUTICS, INC.; AXSOME MALTA LTD.
To: WILMINGTON TRUST, NATIONAL ASSOCIATION
Reel/Frame 071247/0836 →
RELEASE OF SECURITY INTEREST Recorded May 6, 2025
From: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS SUCCESSOR IN INTEREST TO U.S. BANK NATIONAL ASSOCIATION
To: JAZZ PHARMACEUTICALS IRELAND LIMITED
Reel/Frame 071034/0467 →
SECURITY INTEREST Recorded Sep 9, 2024
From: AXSOME MALTA LTD
To: HERCULES CAPITAL, INC.
Reel/Frame 068900/0023 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 16, 2022
From: JAZZ PHARMACEUTICALS IRELAND LIMITED
To: AXSOME MALTA LTD.
Reel/Frame 060223/0878 →
SECURITY AGREEMENT Recorded May 5, 2021
From: CAVION, INC.; CELATOR PHARMACEUTICALS, INC.; JAZZ PHARMACEUTICALS IRELAND LIMITED; JAZZ PHARMACEUTICALS, INC.
To: U.S. BANK NATIONAL ASSOCIATION
Reel/Frame 056151/0010 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 7, 2019
From: HURLEY, FIONN
To: JAZZ PHARMACEUTICALS IRELAND LIMITED
Reel/Frame 050636/0903 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 7, 2019
From: NELSON, JENNIFER LEIGH
To: AMRI SSCI, LLC
Reel/Frame 050636/0946 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 7, 2019
From: AMRI SSCI, LLC
To: JAZZ PHARMACEUTICALS IRELAND LIMITED
Reel/Frame 050641/0673 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 3, 2019
From: JAZZ PHARMACEUTICALS INTERNATIONAL III LIMITED
To: JAZZ PHARMACEUTICALS IRELAND LIMITED
Reel/Frame 049666/0456 →