Novel process for production of highly pure polymorph (i)...

C - Chemistry – Metallurgy – 07 – D

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C07D 211/02 (2006.01) C07D 211/32 (2006.01)

Patent

CA 2630512

The present invention provides a novel, industrially realisable and economically preferable process for production of highly pure l-benzyl-4-[(5,6- dimethoxy-l-indanon)-2-yl]methyl piperidine hydrochloride, i.e., donepezil hydrochloride shown in the following reaction scheme, in Polymorph (I) morphological crystal form. (I) In one of the key steps of the process, during the hydrogenation 5,6-dimethoxy-2-(pyridine-4-yhnethylene)indan-l-one hydrochloride is saturated using Pd carbon to get 4-[(5,6-dimethoxy-l-indanon)- 2-yl]-methyl piperidine at more than 97 % HPLC purity. In the crystallization step donepezil-hydrochloride is crystallized from an aqueous alcoholic solvent to get Polymorph (I) in at least 99.95 % HPLC purity.

La présente invention concerne un nouveau procédé industriellement réalisable et économiquement préférable pour la production de chlorhydrate de 1-benzyl-4-[(5,6-diméthoxy-1-indanon)-2-yl]méthylpipéridine, c'est-à-dire de chlorhydrate de donépézil, extrêmement pur, représenté dans le schéma de réaction suivant, sous la forme de cristaux morphologiques polymorphes (I). (I) Dans une des étapes clés du procédé, au cours de l'hydrogénation, le chlorhydrate de 5,6-diméthoxy-2-(pyridin-4-ylméthylène)indan-1-one est saturé en utilisant du Pd sur carbone pour obtenir de la 4-[(5,6-diméthoxy-1-indanon)-2-yl]méthylpipéridine à plus de 97 % de pureté telle que déterminée par HPLC. Dans l'étape de cristallisation le chlorhydrate de donépézil est cristallisé dans un solvant alcoolique aqueux pour obtenir le polymorphe (I) ayant une pureté d'au moins 99,95 % telle que déterminée par HPLC.

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