Crystallization processes for the formation of stable...

C - Chemistry – Metallurgy – 07 – K

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C07K 5/075 (2006.01) C07K 5/072 (2006.01)

Patent

CA 2348021

A crystallization process for forming a stable crystal of N-(3,3- dimethylbutyl)-APM, which comprises using either water or a mixture of water with a lower alcohol as the crystallizing solvent and controlling the crystallization point to 30 ~C or above; and another crystallization process therefor, which comprises using either water or a mixture of water with a lower alcohol as the crystallizing solvent and using as the seed crystal a crystal of N-(3,3-dimethylbutyl)-APM exhibiting peculiar peaks of diffracted X- ray at least at diffraction angles (2.theta., CuK.alpha. ray) of 6.0~, 24.8~, 8.2~ and 16.5~ to thereby crystallize the above objective crystal preferentially. These crystallization processes enable the constant formation of stable crystals of N-(3,3-dimethylbutyl)-APM at a low cost.

L'invention concerne un procédé de cristallisation pour la formation d'un cristal stable de N-(3,3-diméthylbutyl)-APM, qui consiste à utiliser de l'eau ou un mélange d'eau et d'un alcool inférieur en tant que solvant de cristallisation, et à porter le point de cristallisation à 30 ·C ou plus. L'invention concerne également un autre procédé de cristallisation prévu à cet effet, qui consiste à utiliser de l'eau ou un mélange d'eau et d'un alcool inférieur en tant que solvant de cristallisation, et à utiliser comme cristal germe, un cristal de N-(3,3-diméthylbutyl)-APM présentant des pointes spécifiques de rayon X diffracté, au moins selon des angles de diffraction (rayon CuK.alpha., 2.theta.) de 6,0·, de 24,8·, de 8,2· et de 16,5·, de sorte que le cristal susmentionné soit formé par cristallisation. Ces procédés de cristallisation permettent la formation constante de cristaux stables de N-(3,3-diméthylbutyl)-APM à faible coût.

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