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Uloric crystal and preparation method thereof

A technology of febuxostat and crystal form, which is applied in the field of α crystal form of febuxostat and its preparation, can solve the problem of different solubility, melting point, and dissolution bioavailability, which affect drug stability, bioavailability and curative effect and other problems, to achieve the effect of stable crystal shape, good solubility and simple process operation

Active Publication Date: 2010-03-17
CHINA PHARM UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Different crystal forms of the same drug may have significant differences in appearance, solubility, melting point, dissolution rate, bioavailability, etc., thus affecting the stability, bioavailability and efficacy of the drug

Method used

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  • Uloric crystal and preparation method thereof
  • Uloric crystal and preparation method thereof
  • Uloric crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of febuxostat α crystal form:

[0021] Put 1 g of febuxostat in a 100 ml single-necked flask, add 70 ml of ethylene glycol monomethyl ether, heat and stir in an oil bath at 60°C until completely dissolved. Extract the solvent under reduced pressure at 60°C for crystallization, wash with water, filter, and dry under reduced pressure at 60°C for 8 hours to obtain crystalline powder. Determination of its powder diffraction pattern see figure 1 , see the infrared spectrum figure 2 , according to the powder diffraction pattern and infrared spectrum, it is obvious that the crystalline form α is generated. Yield: 90%, mp: 198-200°C.

Embodiment 2

[0023] Stability test of febuxostat α crystal form

[0024] The α crystal of febuxostat prepared in Example 1 was respectively placed under the conditions of 4500LX, 60°C and RH92.5%, and samples were taken on day 0, day 5, and day 10 for content determination and relevant room determination, and X was drawn - powder diffraction pattern and infrared absorption spectrogram, the results are shown in Table 1.

[0025] The condition and the method of content determination are: high performance liquid chromatography, with methanol-0.01mol / L potassium dihydrogen phosphate solution (75:25) adjust pH value to 5.4 ± 0.1 with 5% phosphoric acid as mobile phase; Detection wavelength λ= 315nm; the preparation of the test solution and the reference solution: accurately weigh about 30mg of the fine powder of the sample, put it in a 100ml measuring bottle, add mobile phase to ultrasonic to dissolve, add mobile phase to the scale, shake well, accurately measure 10ml, put In a 100ml measuring...

Embodiment 3

[0031] Solubility test of febuxostat α crystal form and A crystal form

[0032] The febuxostat α crystal and A crystal were fully ground respectively, and prepared saturated solutions with water, 0.1N HCl, PH5.0 phosphate buffer solution and PH6.8 phosphate buffer solution (ultrasound for 30 minutes, there was still a white solid in the solution substance exists), the content of febuxostat in the saturated solution was determined by ultraviolet spectrophotometry, and the results are shown in Table 2. It can be seen from Table 2 that the solubility of the α crystal form is about double that of the A crystal form.

[0033] Table 2 α crystal form and A crystal form solubility test results

[0034]

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Abstract

The invention relates to the field of medicinal chemistry, in particular to an Uloric crystal and a preparation method thereof. The Uloric crystal is characterized in that x-ray powder diffraction feature absorption peak (2theta) values have feature peaks at the parts of 6.70 degrees, 7.26 degrees, 9.40 degrees, 12.86 degrees, 13.42 degrees, 16.48 degrees, 19.70 degrees, 22.10 degrees, 23.16 degrees, 23.86 degrees, 25.02 degrees, 25.92 degrees, 26.74 degrees, 28.34 degrees and 40.48 degrees. An Uloric alpha crystal form of the invention has simple process operation and low cost. Only Uloric needs to be dissolved in a single solvent of ethylene glycol monomethyl ether so as to avoid solvation crystal habit, and the crystal form is stable and has good reproducibility. Moreover, the Uloric alpha crystal form has good solubility and better dissolution rate than A crystals in a solid preparation.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to an alpha crystal form of febuxostat and a preparation method thereof. Background technique [0002] Febuxostat is a specific xanthine oxidase inhibitor. Compared with allopurinol, febuxostat has similar curative effect and incidence of adverse drug reactions in preventing gout attacks, but has a higher intensity of inhibiting uric acid production. Its chemical name is 2-(3-cyano-4-isobutoxyphenyl)-4-methyl-5-thiazolecarboxylic acid has the activity of inhibiting xanthine oxidase. [0003] [0004] The same substance has two or more spatial arrangements and unit cell parameters, and the phenomenon of forming multiple crystal forms is called polymorphism, and many crystalline drugs have polymorphism. Different crystal forms of the same drug may have significant differences in appearance, solubility, melting point, dissolution rate, bioavailability, etc., thus affecting the st...

Claims

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Application Information

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IPC IPC(8): C07D277/56
Inventor 朱雄黄金龙王越吴葆金殷之武刘嵘
Owner CHINA PHARM UNIV
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