IP Library Granted Patent US 8,901,352
Granted Patent B2
US 8,901,352 · App. 13/979,028 · Granted Dec 2, 2014

Method for the synthesis of rasagiline

Inventors: Ömer Reis (Düzce, TR); Hasan Koyuncu (Düzce, TK); Ilker Esiringu (Düzce, TK); Yasemin Sahin (Düzce, TK); H. Ozan Gulcan (Düzce, TK)
Assignee: Nobel Ilaç Sanayii Ve Ticaret A.S.
C07C209/62C07C233/06C07B2200/07C07C2102/08C07C233/11
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Quick Facts
Patent No.
US 8,901,352
App. No.
13/979,028
Granted
Dec 2, 2014
Kind
B2
Abstract

We have developed a new method for the synthesis of Rasagiline (Formula 1) based on the alkylation of trifluoroacetyl protected aminoindan. This protection enabled us to carry out an alkylation of aminoindan with a high yield and purity under very mild conditions with a wide range of reaction conditions and reagent selection. Considering the ease, purity and high yields of introducing and removal of the trifluoroacetyl group, this approach is a highly practical and economical way for the synthesis of rasagiline or its pharmaceutically acceptable salts.

Claims (21)

1. A compound of Formula 4 or a salt thereof,

2. A process for the preparation of a compound of Formula 1 or a salt thereof, said process comprising the steps of;

(a) alkylating a protected amide compound of Formula 3

with a compound of Formula 6 or an alkylating reagent that can be transformed into an alkyne,

in the presence of a base to obtain a compound of Formula 4

(b) hydrolyzing the compound of Formula 4 to obtain the compound of Formula 1 or a salt thereof.

3. The process according to the claim 2 , wherein the protected amide compound of Formula 3 is obtained by reacting a compound of Formula 2 with a trifluoroacetyl donating group

4. The process according to claim 2 , wherein the alkylating reagent used in the reaction is a compound of Formula 6.

5. The process according to claim 2 , wherein step (a) is carried out in the presence of a base selected from the group consisting of NaOtBu, KOtBu, Cs 2 CO 3 , and a mixture of Cs 2 CO 3 and K 2 CO 3 .

6. The process according to claim 2 , wherein step (a) is carried out in the presence of a phase transfer catalyst.

7. The process according to claim 6 , wherein the phase transfer catalyst is TBAI.

8. The process according to claim 2 , wherein step (a) is carried out in a solvent.

9. The process according to claim 8 , wherein the solvent is DMF or acetonitrile.

10. The process according to claim 2 , wherein step (b) is carried out in a solvent.

11. The process according to claim 2 , wherein step (b) is carried out with a base.

12. The process according to claim 2 , wherein the salt is a mesylate salt of Formula 1.

13. The process according to claim 2 , wherein said process is carried out in one pot.

14. The process according to claim 3 , wherein said process is carried out in one pot.

15. The process according to claim 2 , wherein said alkylating reagent that can be transformed into an alkyne is a compound of Formula 7 or Formula 8

16. The process according to claim 2 , further comprising step (c) converting the compound of the Formula 1 to its salt.

17. The compound of claim 1 wherein said compound is in a racemic mixture.

Assignments (2)
CHANGE OF NAME Recorded Oct 17, 2014
From: FARGEM FARMASÖTIK ARASTIRMA GELISTIRME MERKEZI SANAYI VE TICARET A.S.
To: NOBEL ILAÇ SANAYII VE TICARET A.S.
Reel/Frame 034014/0263 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 24, 2013
From: REIS, OMER; KOYUNCU, HASAN; ESIRINGU, ILKER; SAHIN, YASEMIN; GULCAN, H. OZAN
To: FARGEM FARMASOTIK ARASTIRMA GELISTIRME MERKEZI SANAYI VE TICARET A.S.
Reel/Frame 031270/0848 →
Continuity (1)
Related Publication 20140018578A1 · Jan 16, 2014