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Disclosed are various crystalline salt forms of Boc-D-Arg-DMT-Lys(Boc)-Phe-NH2.

Titel:	CRYSTALLINE SALT FORMS OF BOC-D-ARG-DMT-LYS-(BOC)-PHE-NH2
Link:	View record in USPTO Patent Applications (Volltext)
Veröffentlichung:	2024
Medientyp:	Patent
Sonstiges:	Nachgewiesen in: USPTO Patent Applications Sprachen: English Document Number: 20240140990 Publication Date: May 2, 2024 Appl. No: 18/231483 Application Filed: August 08, 2023 Claim: 1-16. (canceled) Claim: 17. A crystalline form of the freebase of Compound (I), [chemical expression included] (Boc)-D-Arg-DMT-Lys(Boc)-Phe-NH2). Claim: 18. The crystalline form of claim 17, wherein said crystalline form is characterized by an endothermic event in its thermogravimetry differential thermal analysis at an onset of about 168.5° C. Claim: 19. The crystalline form of claim 17, wherein said crystalline form is characterized by an endothermic event in its thermogravimetry differential thermal analysis at a peak at about 175.9° C. Claim: 20. A method of preparing a crystalline form of the freebase of Compound (I), the method comprising: [chemical expression included] a) preparing a mixture comprising the freebase of Compound (I) and a solvent; and b) crystallizing the freebase of Compound (I) from the mixture. Claim: 21. The method of claim 20, wherein the solvent is selected from methanol, ethanol, or trifluoroethanol. Claim: 22. The method of claim 21, wherein the solvent is methanol. Claim: 23. The method of claim 20, wherein the mixture is a solution, and the step of crystallizing the freebase of Compound (I) from the mixture comprises adding an anti-solvent at a temperature, thereby causing the freebase of Compound (I) to precipitate. Claim: 24. The method of claim 23, wherein the ratio of the solvent to the anti-solvent in the solution is about 3:1 to about 1:3. Claim: 25. The method of claim 23, wherein the ratio of the solvent to the anti-solvent in the solution is about 3:1. Claim: 26. The method of claim 23, wherein the ratio of the solvent to the anti-solvent in the solution is about 1:3. Claim: 27. The method of claim 23, wherein the crystallization temperature is about 5 to about 50° C. Claim: 28. The method of claim 23, wherein the crystallization temperature is about 50° C. Claim: 29. The method of claim 23, wherein the crystallization temperature is about 5° C. Claim: 30. The method of claim 23, wherein the anti-solvent is selected from acetonitrile, ethyl acetate, tetrahydrofuran, acetone, methyl ethyl ketone, toluene, tert-butyl methyl ether, and heptane. Claim: 31. A method of making Compound (II), the method comprising deprotecting a crystalline form of the freebase of compound (I), [chemical expression included] thereby making compound (II) [chemical expression included] Claim: 32. The method of claim 31, wherein the step of deprotecting comprises: a. preparing a mixture of a crystalline form of the freebase of compound (I), triisopropylsilane, and 2,2,2-trifluoroethanol; and b. adding concentrated hydrochloric acid to the mixture. Claim: 33. The method of claim 32, wherein the mixture is a slurry. Claim: 34. The method of claim 33, further comprising isolating compound (II) from the mixture. Current International Class: 07; 30

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CRYSTALLINE SALT FORMS OF BOC-D-ARG-DMT-LYS-(BOC)-PHE-NH2