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Roflumilast crystal form compound, preparation method, composition and applications thereof

A technology of roflumilast, compounds, applied in the field of pharmaceuticals to achieve good dissolution, good quality, heat and humidity stability

Active Publication Date: 2013-04-03
天津康鸿医药科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Patent documents with publication numbers WO2005026095A1, WO2004080967A1, US2009171096A1, and CN101490004A all disclose the synthesis and preparation methods of roflumilast, but so far there are no literature reports and patent disclosures related to crystal form data

Method used

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  • Roflumilast crystal form compound, preparation method, composition and applications thereof
  • Roflumilast crystal form compound, preparation method, composition and applications thereof
  • Roflumilast crystal form compound, preparation method, composition and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 1400ml of ethanol to 140g of roflumilast crude product, heat to 80°C and stir to dissolve, hot filter, add 140ml of pure water to the filtrate, stir evenly, place in a refrigerator at 5°C for crystallization, cool for 4h, filter, wash with ethanol, and vacuum dry at 40°C After vacuum drying for 24 hours, 125 g of white roflumilast crystals were obtained.

Embodiment 2

[0033] Add 40ml of methanol to 5g of roflumilast crude product, heat to 75°C and stir to dissolve, hot filter, add 5ml of pure water to the filtrate, stir evenly, place in a refrigerator at 5°C for crystallization, cool for 4h, filter, wash with methanol, and dry in a vacuum oven at 40°C After vacuum drying for 24 hours, 4.5 g of white roflumilast crystals were obtained.

Embodiment 3

[0035] Add 200ml of isopropanol to 27g of roflumilast crude product, heat to 82°C and stir to dissolve, hot filter, add 20ml of pure water to the filtrate, stir evenly, place in a refrigerator at 5°C for crystallization. After cooling for 4 hours, filter, wash with methanol, and dry in a vacuum oven at 40°C for 24 hours to obtain 23 g of white roflumilast crystals.

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PUM

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Abstract

The present invention provides a new roflumilast crystal form compound, wherein an organic solvent and water mixed system is adopted to prepare the compound, and a high yield and good quality are obtained. The specific operation steps comprise: adopting a hot-dissolution cold-precipitation refinement method generally used by technicians in the field to dissolve a roflumilast crude product in an organic solvent solution, heating to a reflux temperature to dissolve, carrying out hot filtration, cooling the filtrate, adding water, precipitating a crystal, filtering, and carrying out vacuum drying.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular, the invention relates to a crystal form compound of roflumilast, a preparation method of the crystal form compound, a pharmaceutical composition containing the crystal form compound and applications thereof. Background technique [0002] Chronic obstructive pulmonary disease (COPD) is a serious lung disease that makes breathing difficult. Symptoms can include shortness of breath, chronic cough, and excess phlegm. A bout of illness can last for weeks and lead to reduced lung function, increased risk of death, and can be accompanied by severe anxiety. Research results of the American Heart, Lung, and Blood Institute show that smoking is the main cause of COPD; in the United States, COPD is the fourth leading cause of death from diseases. [0003] Conventional treatment of COPD is basically symptomatic relief of bronchodilation with inhaled anticholinergics and inhaled β2-adrenoceptor ago...

Claims

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Application Information

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IPC IPC(8): C07D213/75A61K31/44A61P11/06A61P11/00
Inventor 韩学文邹美香张晓军吴疆王杏林孙歆慧
Owner 天津康鸿医药科技发展有限公司
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