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

A technology of citric acid and amorphous form, which is applied in the field of edenafil citrate crystal form D and its preparation and application, and can solve problems not related to edenafil citrate crystal form and its preparation method

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 edenafil citrate crystal form and its preparation method

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0094] In a 100ml reaction bottle, add 3 grams of edenafil citrate, 85ml of distilled water / absolute ethanol (50:50, volume ratio), start stirring, heat up to reflux temperature, filter while hot after 15 minutes, and seal the container Put the filtrate in a filter bottle, place it indoors, lower the temperature naturally to 30°C-35°C, keep it warm for 58 hours, precipitate crystals, filter, place it indoors for 1 hour, and dry to obtain the crystalline form of aldenafil citrate D 1.8g, its melting point is m.p 201.9-203.1°C, the refining rate is 60%, and the content measured by HPLC area normalization method is 99.92%. See figure 1 , figure 2 , image 3 and Image 6 , is the three-dimensional structure projection diagram, unit cell projection diagram, infrared spectrum diagram and X-ray powder diffraction diagram of aldenafil crystal form D citrate molecule, showing the characteristics of aldenafil crystal form D citrate.

Embodiment 2

[0096] In a 200ml reaction bottle, add 5 grams of edenafil citrate, 160ml of distilled water / absolute ethanol (40:60, volume ratio), start stirring, heat up to reflux temperature, filter while it is hot after 15 minutes, and seal it. Put the filter bottle of the filtrate, place it indoors, cool down naturally to 30°C-35°C, keep it warm for 65 hours, precipitate crystals, filter, place it indoors for 1 hour, and dry to obtain Aldenamorph citrate crystal form D 2.8g, its melting point is m.p 201.9-203.1°C, the refining rate is 56%, and the content measured by HPLC area normalization method is 99.92%. After testing, it showed the characteristics of edenamorph citrate crystal form D.

Embodiment 3

[0098] Granules Containing Aldenafil Citrate Form D

[0099] Prescription: 50 grams of Aldenafil Citrate Form D, 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.

[0100] Process: PEG-4000 and aldenamorph citrate crystal form D 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 packaged into granules.

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Abstract

The invention relates to 1-[3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazole parallel [4, 3-d] pyridine-5-thyl)-4-ethoxylbenzene sulfonyl]-cis-3, 5-lupetazin citrate or citric acid alidenafil crystal form D and preparation method thereof and also relates to drug combination containing citric acid alidenafil crystal form D and application thereof in preparation of drug for treating erection disturbance. Citric acid alidenafil raw material is dissolved in distilled water/acetone mixed solution in certain proportion, and heat preservation is carried out for 50-72 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 D is obtained, the crystal form D can form a combination 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)- 4-ethoxybenzenesulfonyl]-cis-3,5-dimethylpiperazine citrate (Aildenafil citrate) crystal form D, and its preparation method, containing the present invention The pharmaceutical composition of the obtained crystal form D and the application of the crystal form D in the manufacture of a drug for treating male erectile dysfunction (male erectile dysfunction, ED). 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 m...

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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