Method for crystallization of 2-amino-2-[2-[4-(3-...

C - Chemistry – Metallurgy – 07 – C

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C07C 319/28 (2006.01) A61K 31/145 (2006.01) A61P 37/00 (2006.01) B01D 9/02 (2006.01) C07C 323/32 (2006.01)

Patent

CA 2718987

The present invention herein provides a method for highly efficiently preparing high purity crystals of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chloro- phenyl]-ethyl]-1, 3-propane diol hydrochloride. The method comprises the following steps: (1) dissolving 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]- 1, 3-propanediol in a mixed solvent comprising a solvent in which the compound in the form of the hydrochloride thereof is highly soluble and a solvent in which the compound in its hydrochloride is less soluble, to thus prepare a solution of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]ethyl]-1,3-propane diol; and then (2) adding hydrochloric acid to the resultant solution with stirring, to thus crystallize the hydrochloride of 2-amino-2-[2-[4-(3-benzyloxyphenylthio)-2-chloro-- phenyl]ethyl]-1, 3-propanediol.

L'invention porte sur un procédé de fabrication d'un cristal extrêmement pur de chlorhydrate de 2-amino-2-[2-[4-(3-benzyloxyphénylthio)-2-chlorophényl]éthyl]-1,3-propanediol avec un rendement élevé. Le procédé comprend les étapes (1) et (2) suivantes : (1) la dissolution de 2-amino-2-[2-[4-(3-benzyloxyphénylthio)-2-chlorophényl]éthyl]-1,3-propanediol dans un solvant mélangé composé d'un solvant ayant une solubilité élevée pour le chlorhydrate de 2-amino-2-[2-[4-(3-benzyloxyphénylthio)-2-chlorophényl]éthyl]-1,3-propanediol et d'un solvant ayant une médiocre solubilité pour le chlorhydrate de 2-amino-2-[2-[4-(3-benzyloxyphénylthio)-2-chlorophényl]éthyl]-1,3-propanediol pour préparer une solution de 2-amino-2-[2-[4-(3-benzyloxyphénylthio)-2-chlorophényl]éthyl]-1,3-propanediol; et (2) l'ajout d'acide chlorhydrique à la solution tout en agitant la solution pour provoquer la cristallisation de chlorhydrate de 2-amino-2-[2-[4-(3-benzyloxyphénylthio)-2-chlorophényl]éthyl]-1,3-propanediol.

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