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More stable doxofylline compound and pharmaceutical composite thereof

A technology for doxofylline and compound, applied in the field of preparation of pharmaceutical compounds, can solve problems such as more than 0.2%, and achieve the effects of long standing time, high yield and reduced impurity content

Inactive Publication Date: 2012-03-07
河北三禾实创生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the prior art uses 95% ethanol as the recrystallization solvent. Although the content of doxofylline after recrystallization is greater than 99%, the content of two related impurities with unknown structures is greater than 0.2%.

Method used

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  • More stable doxofylline compound and pharmaceutical composite thereof
  • More stable doxofylline compound and pharmaceutical composite thereof
  • More stable doxofylline compound and pharmaceutical composite thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The doxofylline crude product is dissolved in a mixed solvent of ethyl acetate and methanol=1:2 (v / v) with 8 times its weight, and the gac of about 5% (v / w) weight of the solution volume is added, heated to reflux temperature, continued for 1 hour, placed at room temperature for 24 hours, crystallization was precipitated, crystallization was obtained after suction filtration, and the above steps were repeated to obtain the second recrystallization product, which was washed with ethyl acetate and dried to obtain the pure product of doxofylline. HPLC detection shows that the pure product of doxofylline has a purity of 99.85%, and the content of unknown impurities is less than 0.1%.

Embodiment 2

[0045] The doxofylline pure product 100g that embodiment 1 obtains

[0046] Sodium bisulfite 10g

[0047] Edetate Disodium 5g

[0048] PEG-400 50g

[0049] Disodium hydrogen phosphate-sodium dihydrogen phosphate buffer 10L

[0050] Its preparation method is as follows:

[0051] Get doxofylline 100g, mix and grind with PEG-400, dissolve the ground material of doxofylline and PEG-400 with the prepared disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution with a pH value of 6.5, add 0.5% activated carbon, heated to 80°C and maintained for 15 minutes, filtered to remove carbon, then added sodium bisulfite, disodium edetate, stirred to dissolve, added disodium hydrogen phosphate-sodium dihydrogen phosphate buffer to 10000ml, added 0.5% activated carbon, boiled, finely filtered with a 0.45 μm microporous membrane, and sterilized with a 0.20 μm microporous membrane, canned, sterilized, and labeled.

Embodiment 3

[0053] Doxofylline 100g

[0054] Sodium bisulfite 10g

[0055] Edetate Disodium 5g

[0056] PEG-400 50g

[0057] Disodium hydrogen phosphate-sodium dihydrogen phosphate buffer 10L

[0058] Its preparation method is as follows:

[0059]Get doxofylline 100g, mix and grind with PEG-400, dissolve the ground material of doxofylline and PEG-400 with the prepared disodium hydrogen phosphate-sodium dihydrogen phosphate buffer solution with a pH value of 6.5, add 0.5% activated carbon, heated to 80°C and maintained for 15 minutes, filtered to remove carbon, then added sodium bisulfite, disodium edetate, stirred to dissolve, added disodium hydrogen phosphate-sodium dihydrogen phosphate buffer to 10000ml, added 0.5% activated carbon, boiled, finely filtered with a 0.45 μm microporous membrane, and sterilized with a 0.20 μm microporous membrane, canned, semi-sealed, put into a freeze-drying box, freeze-dried, sealed, Label it and pack it.

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Abstract

The invention relates to a more stable doxofylline compound and a pharmaceutical composite thereof. The preparation method of the doxofylline compound comprises the following steps: recrystallizing crude doxofylline with a mixed solvent of ethyl acetate and methanol for 1-3 times and decoloring with activated carbon to obtain off-white crystals, wherein the ratio of ethyl acetate to methanol is 1:2.

Description

Technical field: [0001] The invention relates to the preparation of a medicinal compound, especially the antiasthmatic drug doxofylline compound. Background technique: [0002] Doxofylline, a derivative of methylxanthine, is a bronchodilator that acts directly on the bronchi to relax bronchial smooth muscle. By inhibiting the action of phosphodiesterase in smooth muscle cells, it relaxes smooth muscle, thereby achieving the effect of inhibiting asthma. [0003] Common name: doxofylline, English name: Doxofylline, chemical name: 1,3-dimethyl-7-(1,3-dioxol-2-yl)methyl-3,7-di Hydrogen-1H-purine-2,6-dione. The structural formula is: [0004] [0005] The product has injections and oral preparations, and its pharmacokinetic parameters are: patients with chronic bronchitis receive 100 mg of doxofylline intravenously (injection time exceeds 10 minutes), and the plasma drug peak time (tmax) after administration is about 0.10 hours, The peak plasma concentration (Cmax) is abou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/08A61K31/522A61K9/19A61K9/08
Inventor 贺金凤
Owner 河北三禾实创生物科技有限公司
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