Doxofylline crystalline compound and lyophilized powder thereof

A technology of doxofylline and freeze-dried powder injection, applied in the field of medicine

Inactive Publication Date: 2013-06-12
SHANXI PUDE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, doxofylline did not produce typical cardiovascular and cereb

Method used

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  • Doxofylline crystalline compound and lyophilized powder thereof
  • Doxofylline crystalline compound and lyophilized powder thereof
  • Doxofylline crystalline compound and lyophilized powder thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 Preparation of doxofylline crystalline compound

[0035] (1) Take 10 g of commercially available doxofylline crude product and fully dissolve it in 45 ml of a mixed solution of water / n-butanol / acetonitrile with a volume ratio of 4:3:1.5, heat to reflux, stir and dissolve to obtain a doxofylline solution ;

[0036] (2) Add dropwise 9ml of ether / methanol solution with a volume ratio of 4:1 to the doxofylline solution under reflux and stirring, and finish dropping in 8-10 minutes;

[0037] (3) Stop heating, stir at a rotating speed of 50rmp and cool down to 10°C, wherein the cooling rate is 8°C / 5min, stand still for 18h to crystallize, filter, wash the filter cake with 5ml of ether, and vacuum-dry the crystalline compound of doxofylline, Yield 88.5%, HPLC 99.54%, mp 178~181℃.

[0038] The described doxofylline crystalline compound is measured by powder X-ray diffractometry, and the X-ray powder diffraction spectrum represented by 2θ ± 0.2° diffraction angle is ...

Embodiment 2

[0039] Example 2 Preparation of doxofylline crystalline compound

[0040] (1) Take 10 g of commercially available doxofylline crude product and fully dissolve it in 55 ml of a mixed solution of water / n-butanol / acetonitrile with a volume ratio of 4:3:1.5, heat to reflux, stir and dissolve to obtain a doxofylline solution ;

[0041] (2) Add dropwise 7ml of ether / methanol solution with a volume ratio of 4:1 to the doxofylline solution under reflux and stirring, and the dripping will be completed within 8 to 10 minutes;

[0042] (3) Stop heating, stir at a rotating speed of 30rmp and cool down to 5°C, wherein the cooling rate is 5°C / 5min, let it stand for 24h to crystallize, filter, wash the filter cake with 5ml of ether, and vacuum-dry the crystalline compound of doxofylline, Yield 88.7%, HPLC 99.50%, mp178~181℃.

[0043] The described doxofylline crystalline compound is measured by powder X-ray diffractometry, and the X-ray powder diffraction spectrum represented by 2θ ± 0.2° ...

Embodiment 3

[0044] Example 3 Preparation of doxofylline crystalline compound

[0045] (1) Take 10 g of commercially available doxofylline crude product and fully dissolve it in 50 ml of a mixed solution of water / n-butanol / acetonitrile with a volume ratio of 4:3:1.5, heat to reflux, stir and dissolve to obtain a doxofylline solution ; Add 2g of activated carbon, reflux for 0.5h, filter, and collect the filtrate;

[0046](2) Add 8ml of ether / methanol solution with a volume ratio of 4:1 to the filtrate of step (1) dropwise under reflux and stirring, and it will be dripped within 8 to 10 minutes;

[0047] (3) Stop heating, stir at a rotating speed of 40rmp and cool down to 8°C, wherein the cooling rate is 6.5°C / 5min, let stand for 20h to crystallize, filter, wash the filter cake with 5ml of ether, and vacuum-dry the crystalline compound of doxofylline, Yield 88.3%, HPLC 99.79%, mp179~181℃.

[0048] The described doxofylline crystalline compound is measured by powder X-ray diffractometry, an...

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PUM

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Abstract

The invention relates to a doxofylline crystalline compound and lyophilized powder thereof. The doxofylline crystalline compound is measured by a powder X-ray diffraction measurement method; and an X-ray powder diffraction pattern represented by a diffraction angle of 2(theta)+/-0.2 degrees shows characteristic diffraction peaks at the positions of 10.21 degrees, 12.12 degrees, 14.39 degrees, 23.32 degrees, 24.43 degrees, 27.23 degrees, 28.60 degrees, 30.54 degrees, 32.28 degrees, 33.32 degrees, 34.38 degrees and 36.12 degrees. The re-dissolubility of the doxofylline crystalline compound provided by the invention is obviously improved, solid is not easily separated out after long-time placement, and the medication safety of a patient is greatly improved.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a doxofylline crystalline compound and its freeze-dried powder injection. Background technique [0002] The death rate of respiratory diseases ranks first among all diseases. Among respiratory diseases, chronic obstructive pulmonary disease (COPD) such as bronchial asthma, chronic bronchitis and emphysema is the most common. Asthma is the most common chronic disease in Western countries. Asthma causes the muscles in the airways to become overly tense, making it difficult to breathe. Its morbidity and mortality are increasing year by year. According to statistics, COPD in my country causes about 1 million deaths and 5-10 times the number of disabilities every year (doxofylline is a safe and effective drug for the treatment of chronic obstructive pulmonary disease); the national epidemiological survey in 2000 showed , the prevalence of asthma is 0.25-4.63%, more than doubled over the last...

Claims

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Application Information

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IPC IPC(8): C07D473/08A61K9/19A61K31/522A61P11/08A61P11/06A61P11/00
Inventor 王勇李立忠解晓荣李润宝昝建强姚荷云闫洁胡成伟
Owner SHANXI PUDE PHARMA CO LTD
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