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Doxofylline hemihydrate

A technology of doxofylline and hydrate, which is applied in the field of doxofylline hemihydrate and its preparation, can solve the problem that the amount of impurities cannot be effectively controlled, there are many types of impurities, and there is no refining method for doxofylline hemihydrate. Detailed research and disclosure of issues to achieve the effect of reducing market risk, high solubility, and simple methods

Active Publication Date: 2014-01-22
天津梅花生物医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0020] During the research process, repeating the method of the above-mentioned patent documents, the crude product of doxofylline obtained has many types of impurities, and the amount of impurities cannot be effectively controlled. The refining method of doxofylline hemihydrate has not been studied and disclosed in detail.

Method used

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  • Doxofylline hemihydrate

Examples

Experimental program
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Effect test

Embodiment 1

[0057] In a 5000ml reaction bottle equipped with stirring, thermometer and condenser, add 100g of doxofylline, 0.5g of dimethylformamide (DMF) and 1000ml of water-ethanol=1:10 mixture, start stirring, Heat up to 55°C-60°C, heat up to reflux for 1 hour, cool down to room temperature naturally, then cool to 5°C, continue to stir and crystallize for 1 hour, filter, and dry at 50°C for 3 hours under nitrogen atmosphere to obtain doxofylline 90.8 grams of hemihydrate powder, the moisture measured by the Karl Fischer method is 3.33%.

[0058] The X-ray diffraction pattern of the compound is shown in figure 1 . Instrument model and measurement conditions: Rigaku D / max2500 diffractometer; CuKa40Kv100mA; 2θ scanning range: 0-50°.

[0059] The infrared spectrum of the compound is shown in figure 2 , Determination with KBr tablet.

Embodiment 2

[0061] In a 5000ml reaction bottle equipped with stirring, thermometer and condenser, add 100g of doxofylline, 0.5g of dimethylformamide (DMF) and 800ml of water-ethanol=1:8 mixture, start stirring, Heat up to 55°C-60°C, heat up to reflux for 1 hour, cool down to room temperature naturally, then cool to 5°C, continue to stir and crystallize for 1 hour, filter, and dry at 50°C for 3 hours under nitrogen atmosphere to obtain doxofylline 91.8 grams of hemihydrate powders, the moisture measured by the Karl Fischer method is 3.18%.

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Abstract

The invention specifically relates to a doxofylline hemihydrate, which belongs to the field of medical technology. The doxofylline hemihydrate provided by the invention has good stability and has no obvious moisture absorption and weight gain under a high humidity condition, and related substances do not increase; compared with doxofylline in other crystalline states, the doxofylline hemihydrate has high solubility. A preparation method for the doxofylline hemihydrate comprises the following steps: weighing doxofylline, putting weighed doxofylline in a reaction vessel, adding a proper volume of an ethanol aqueous solution, successively carrying out stirring, heating reflux, natural cooling to room temperature and cooling to 5 DEG C, continuing stirring for crystallization for 1 h, carrying out filtering and then carrying out drying at a temperature of 50 DEG C in a nitrogen atmosphere so as to obtain the doxofylline hemihydrate. Chemical purity of the doxofylline hemihydrate reaches 99.9%, and total impurities are less than 0.08%.

Description

technical field [0001] The invention relates to medicines in the field of medicine, in particular to a doxofylline hemihydrate and a preparation method thereof. Background technique [0002] With the global air pollution and environmental deterioration, the morbidity and mortality of asthma are increasing year by year. Experts predict that the anti-asthma drug market will be one of the ten most promising drug markets in the next 20 years. The incidence rate is relatively high in different regions, with Fujian being the highest at 3.03%, followed by Guangdong at 2.53%, and less in the north and inland areas. The incidence of asthma is higher in winter, followed by late autumn and early spring, and the lowest in summer. Bronchial asthma and chronic bronchitis, pulmonary Emphysema and other chronic obstructive pulmonary diseases (COPD) are the most common. Asthma factors are difficult to cure and expensive. Among respiratory diseases, chronic obstructive pulmonary diseases (COP...

Claims

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Application Information

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IPC IPC(8): C07D473/08A61K31/522A61P11/06A61P11/00A61P29/00
CPCC07D473/08
Inventor 梅开忠黄欣
Owner 天津梅花生物医药科技有限公司
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