2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism as well as preparation method, preparation and application thereof

A technology of potassium benzoate and hydroxypentyl, applied in the field of medicine, can solve the problems of differences in physical and chemical properties, the problem of polymorphism not mentioned, affecting the application of drugs and clinical efficacy, etc., and achieve the effect of stable properties and simple preparation methods

Active Publication Date: 2014-07-02
YUNNAN HAOPY PHARM LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent CN1382682A discloses 2-(alpha-hydroxypentyl) potassium salt of benzoate and its preparation method and application, and provides three purification methods of methanol, methanol-chloroform and methanol-ether recrystallization respectively, and all obtain ...

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  • 2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism as well as preparation method, preparation and application thereof
  • 2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism as well as preparation method, preparation and application thereof
  • 2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism as well as preparation method, preparation and application thereof

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Experimental program
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Embodiment 1     —— preparation example

[0067] Embodiment 1——Preparation example: the preparation of 2-(alpha-hydroxypentyl) potassium benzoate medicinal product

[0068] Take 60 grams of crude potassium 2-(α-hydroxypentyl)benzoate, put it in absolute ethanol (1g: 2ml, w / v), heat to reflux to obtain a slightly turbid solution, and filter it while it is hot. The clarified filtrate was placed in the refrigerator after cooling, and white granular crystals were precipitated. The filtered potassium 2-(α-hydroxypentyl)benzoate was recrystallized in absolute ethanol according to the above method, repeated three times until the crystal melting point remained unchanged (mp153~155°C), and a total of 46.8g of white granular crystals were obtained ( Recrystallization yield 78%), this is 2-(α-hydroxypentyl) potassium benzoate pharmaceutical products.

Embodiment 2

[0069] Example 2——Preparation of 2-(α-hydroxypentyl) potassium benzoate crystal form I

[0070] Add 10 g of potassium 2-(α-hydroxypentyl)benzoate medicinal product in Example 1 into about 19 mL of methanol, heat until dissolved, filter while hot, cool to room temperature, and precipitate crystals. After filtering and drying, it was recrystallized once with methanol according to the above method. After drying, 6.5 g of white crystals (recrystallization yield 65%) were obtained, with a melting point of 152-154°C. Carry out powder X-ray diffraction after this crystal is crushed, and the collection of illustrations is shown in the attached figure 1 , see Table 1 for the data.

Embodiment 3

[0071] Example 3——Preparation of 2-(α-hydroxypentyl) potassium benzoate crystal form I

[0072] Add 10 g of potassium 2-(α-hydroxypentyl)benzoate medicinal product in Example 1 into about 20 mL of absolute ethanol, heat to dissolve, filter while hot, cool to room temperature, and precipitate crystals. After filtering and drying, recrystallize once with absolute ethanol according to the above method, and after drying, 6.7 g of white crystals (recrystallization yield 67%) were obtained, with a melting point of 153-155°C. Carry out powder X-ray diffraction after this crystal is crushed, and the collection of illustrations is shown in the attached figure 2 , see Table 1 for the data.

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Abstract

The invention discloses 2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism as well as a preparation method, a preparation and an application thereof. A characteristic diffraction peak is displayed by an X-ray diffraction pattern of the polycrystalline powder at a reflection angle within 2Theta+/-0.1 DEG of 7.0, 20.8 and 26.4+/-0.2 DEG. The preparation method comprises the following step: carrying out crystallization by selecting one or any combination of methyl alcohol, absolute ethyl alcohol, 95% ethyl alcohol, 75% ethyl alcohol, 50% ethyl alcohol and 2-butanol and selecting one or any combination of normal propyl alcohol and isopropyl alcohol or selecting the normal butanol. The preparation is of tablets, capsules, granules, a freeze-dried powder injection and an injection liquid, which is prepared by adding pharmaceutically acceptable carriers and auxiliary materials into the 2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism. The 2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism is applied to a medicine for treating a neurodegenerative disease. The 2-(Alpha-hydroxyl amyl) potassium benzoate polymorphism is stable in performance and suitable for industrial production, thereby laying the foundation for the development of a 2-(Alpha-hydroxyl amyl) potassium benzoate medicine.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a polymorphic form of potassium 2-(α-hydroxypentyl)benzoate and a preparation method, preparation and application thereof. Background technique [0002] Cerebrovascular disease is a disease caused by blockage or rupture of cerebral blood vessels that blocks blood flow in the brain. It is divided into ischemic stroke and hemorrhagic stroke. Epidemiological survey results show that there are about 1.5 to 2 million new stroke patients in my country every year, of which ischemic stroke accounts for about 80% of stroke cases. This incidence rate is not only much higher than the United States and other developed countries, but also higher than the world average. What's more serious is that with the improvement of my country's industrialization level and people's living standards, the incidence of stroke is still on the rise. Stroke not only endangers people's health with...

Claims

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Application Information

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IPC IPC(8): C07C65/01C07C51/41C07C51/43A61K31/192A61P25/28A61P9/10
CPCC07C51/41C07C51/43C07C65/01
Inventor 李彪王涌杨云
Owner YUNNAN HAOPY PHARM LTD
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