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Citric acid alidenafil crystal form B and preparation method and usage thereof

A citric acid, amorphous technology, applied in the field of citrate aldenafil crystalline form B and its preparation and use, can solve the problems that do not involve the citrate aldenafil crystalline form and preparation method and the like

Inactive Publication Date: 2010-03-17
刘桂坤
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent (application number 02100198.7) discloses edenafil and its preparation method, etc., but does not involve the crystal form of edenafil citrate and its preparation method

Method used

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  • Citric acid alidenafil crystal form B and preparation method and usage thereof
  • Citric acid alidenafil crystal form B and preparation method and usage thereof
  • Citric acid alidenafil crystal form B and preparation method and usage thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0091] In a 100ml reaction bottle, add 3 grams of edenafil citrate and 88ml of distilled water, start stirring, heat up to the reflux temperature, filter while it is hot after 15 minutes, seal the filtrate in the filter bottle, place it indoors, and cool down naturally , lowered to 25°C-30°C, kept it for 35 hours, precipitated crystals, filtered, placed indoors for 1 hour, then moved to a vacuum drying oven, and dried in vacuum for 3 hours to obtain the above crystal form of aldenamorph citrate B 2.1g, its melting point is m.p 212.5-215.0°C, and the refining rate is 70%. The content measured by HPLC area normalization method is 99.93%. See Figure 1-Figure 3, It is the molecular three-dimensional structure projection diagram, the unit cell projection diagram and the infrared spectrum diagram of Aldenamorph citrate crystal form B, showing the characteristics of Aldenafil crystal form B citrate.

Embodiment 2

[0093] In a 250ml reaction bottle, add 5 grams of edenafil citrate, 130ml of distilled water, and 0.25 grams of activated carbon, start stirring, heat up to reflux temperature, and filter while hot after 18 minutes. Seal the filtrate in a filter bottle, place it indoors, lower the temperature naturally to 25°C-30°C, keep it warm for 45 hours, precipitate crystals, filter, place it indoors for 1.5 hours, then move it to a vacuum drying oven and dry it in vacuum for 4 Within hours, 3.7 g of the crystalline form B of the edenafil citrate compound was obtained, with a melting point of m.p 212.5-215.0° C. and a purification rate of 74%. The content measured by HPLC area normalization method is 99.93%. After testing, it showed the characteristics of edenamorph citrate crystal form B.

Embodiment 3

[0095] Granules Containing Aldenafil Citrate Form B

[0096] Prescription: 50 grams of Aldenafil Citrate Form B, 650 grams of lactose, 100 grams of crospovidone, 90 grams of PEG-4000, 135 grams of hydroxypropyl methylcellulose, appropriate amount of distilled water, made into 1000 bags.

[0097] Process: PEG-4000 and aldenafil citrate crystal form B are crushed together, passed through an 80-mesh sieve, mixed with other materials, made into soft materials with distilled water, granulated, dried at low temperature, and then packed into granules.

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Abstract

The invention relates to 1-[3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazolo [4, 3-d] pyridine-5-thyl)-4-ethoxylbenzene sulfonyl]-cis-3, 5-lupetazin citrate or citric acid alidenafil crystal form Band preparation method thereof and also relates to drug composistion containing citric acid alidenafil crystal form B and application thereof in preparation of drug for treating erection disturbance(ED). Citric acid alidenafil raw material is dissolved in distilled water in certain proportion, and heat preservation is carried out for 30-48 hours while stirring is carried out at certain temperature, thus obtaining the product. Test by an X-ray powder diffractometer, thermogravimetric analysis and infrared spectrometer proves that an unprecedented citric acid alidenafil crystal form B is obtained, the crystal form B can form a composition with one or multiple pharmaceutically acceptable carrier, excipient or diluent and can be effectively applied to treatment on andropathy.

Description

technical field [0001] The present invention relates to 1-[3-(6,7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazolo[4,3-d]pyrimidin-5-yl)- Crystal form B of 4-ethoxybenzenesulfonyl]-cis-3,5-dimethylpiperazine citrate (Aildenafil citrate), its preparation method, and the The pharmaceutical composition of the obtained crystal form B and the application of the crystal form B in the manufacture of medicines for treating male erectile dysfunction (male erectile dysfunction, ED) are disclosed. Background technique [0002] Male erectile dysfunction (male erectile dysfunction, ED) is a common disease, which can be defined as the inability to erect the penis, ejaculate or both. According to statistics, its incidence rate accounts for 1.9% in men over 40 years old, and the incidence rate is 1.9% in men over 65 years old. For men it reaches 65%. There are about 125 million men in the world suffering from different degrees of erectile dysfunction, and it is expected to reach 322 million by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04A61K31/519A61P15/10
Inventor 刘桂坤
Owner 刘桂坤
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