Method for preparing crystal of...

C - Chemistry – Metallurgy – 07 – C

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C07C 233/65 (2006.01) C07C 231/24 (2006.01) C07C 235/84 (2006.01)

Patent

CA 2420962

A method for preparing a crystal of 4-[(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl- 2-naphthalenyl)carbamoyl]benzoic acid having a single endothermic peak approximately at 233°C in differential scanning calorimetry, which comprises the step of recrystallizing a crystal of 4-[(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2- naphthalenyl)carbamoyl]benzoic acid from a mixture of water and ethanol. The method enables selective preparation of type-Il crystals which are stable against physical impact. The resulting crystals are free from highly toxic hexane as a residual solvent, and preferably used as an active ingredient of pharmaceuticals.

Cette invention a trait à un procédé de production de cristaux d'acide benzoïque 4-[(5,6,7,8-tétrahydro-5,5,8,8-tétraméthyl-2-naphtalényl) carbamoyl] présentant un pic endothermique voisin de 233 DEG C en calorimétrie différentielle à balayage. Ce procédé consiste à recristalliser des cristaux d'acide benzoïque 4-[(5,6,7,8-tétrahydro-5,5,8,8-tétraméthyl-2-naphtalényl) carbamoyl] à partir d'un mélange d'eau et d'alcool éthylique. Ce procédé permet de produire, de manière sélective, des cristaux du type II, stables face aux chocs physiques. Les cristaux ainsi obtenus sont exempts d'un solvant résiduel, en l'occurrence l'hexane, très toxique, ce qui permet de les utiliser au mieux comme ingrédients actifs dans des préparations médicamenteuses.

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