IP Library Granted Patent US 9,657,047
Granted Patent B2
US 9,657,047 · App. 13/471,537 · Granted May 23, 2017

Crystallization of epirubicin hydrochloride

Inventor: Tero Kunnari (Aschaffenburg, DE)
Assignee: MEDAC GESELLSCHAFT FÜR KLINISCHE SPEZIALPRÄPARATE MBH
C07H15/252C07H1/06
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Quick Facts
Patent No.
US 9,657,047
App. No.
13/471,537
Granted
May 23, 2017
Kind
B2
Abstract

A crystalline epirubicin hydrochloride and a method for its production are provided. The method for producing the crystalline epirubicin hydrochloride includes the steps: (a) providing epirubicin hydrochloride, (b) producing a mixture containing the provided epirubicin hydrochloride and at least one alcohol selected from the group 1-butanol, 2-butanol, and 1-pentanol, and (c) crystallizing epirubicin hydrochloride from this mixture.

Claims (15)

1. A method for producing crystalline epirubicin hydrochloride, comprising steps of:

(a) providing epirubicin hydrochloride;

(b) combining the epirubicin hydrochloride provided in step (a), at least one first alcohol selected from the group consisting of 1-butanol, 2-butanol, and 1-pentanol, and at least one second alcohol which is 2-propanol to produce a mixture containing the epirubicin hydrochloride, the at least one first alcohol, the at least one second alcohol and water, the water being provided in step (a) and/or step (b), a proportion of the epirubicin hydrochloride contained in the mixture being in the range of 10-50 g/l relative to the total volume of the mixture; and

(c) crystallizing the epirubicin hydrochloride from the mixture produced in step (b) by heating the mixture produced in step (b) to a temperature in the range of 50-75° C. for a time period of at least 2 hours.

2. The method according to claim 1 , wherein the epirubicin hydrochloride provided in step (a) is contained in a solution.

3. The method according to claim 2 , wherein the solution is an aqueous solution.

4. The method according to claim 3 , wherein the epirubicin hydrochloride provided in step (a) is contained in a proportion of 100-400 g/l, relative to the total volume of the aqueous solution.

5. The method according to claim 1 , wherein the epirubicin hydrochloride provided in step (a) is in crystalline or amorphous form.

6. The method according to claim 1 , wherein the at least one first alcohol is present in the mixture produced in step (b) in a proportion lying in a range of 5-50 volume percent, relative to the total volume of the mixture.

7. The method according to claim 1 , wherein the at least one second alcohol is present in the mixture produced in step (b) in a proportion lying in a range of 5-95 volume percent, relative to the total volume of the mixture.

8. The method according to claim 1 , wherein the ratio of a volume of the second alcohol to a volume of the first alcohol lies in the range of 3:1 to 20:1.

9. The method according to claim 1 , wherein, in step (b), the proportion of the water in the mixture lies in the range of 0.5-7 volume percent, relative to the total volume of the mixture.

10. The method according to claim 1 , wherein a pH value of the mixture produced in step (b) lies in the range of 2.5-4.5.

11. The method according to claim 1 , wherein in step (c) the mixture is left at a temperature in the range of 50-75° C. for a time period of 2-8 hours.

12. The method according to claim 1 , wherein crystals produced in step (c) are separated from the remainder of the mixture.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 7, 2016
From: HERAEUS DEUTSCHLAND GMBH & CO. KG
To: MEDAC GESELLSCHAFT FÜR KLINISCHE SPEZIALPRÄPARATE MBH
Reel/Frame 039659/0523 →
CHANGE OF NAME Recorded Nov 6, 2015
From: HERAEUS PRECIOUS METALS GMBH & CO. KG
To: HERAEUS DEUTSCHLAND GMBH & CO. KG
Reel/Frame 037056/0430 →
Priority Claims (1)
DE 10 2011 103 751 · May 31, 2011 · national
Continuity (2)
Provisional Application 61493034 · Jun 3, 2011
Related Publication 20120309948A1 · Dec 6, 2012