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Citric acid aildenafil crystal form A 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 A and its preparation and application, and can solve problems not related to edenafil citrate crystal form and its preparation method

Active 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 aildenafil crystal form A and preparation method and usage thereof
  • Citric acid aildenafil crystal form A and preparation method and usage thereof
  • Citric acid aildenafil crystal form A and preparation method and usage thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] In a 1000ml reaction bottle, add 30g of edenafil citrate, 480ml of distilled water, and 0.3g of activated carbon, start stirring, heat up to reflux, filter while it is hot after 15 minutes, the filtrate drops to 38°C-42°C, keep stirring 60 minutes, then cool down to room temperature naturally, continue to stir at 20°C-26°C for 11 hours, precipitate crystals, filter, place in the room for 5 hours, then move to a vacuum drying oven, and vacuum dry for 6 hours to obtain the above-mentioned Aldicitrate The amorphous form A is 27g, the refining rate is 90%, and the content is 99.91% measured by HPLC area normalization method, see figure 1- image 3, Detected by X-ray diffractometer, infrared spectrometer and thermal analyzer, it shows the characteristics of edenamorph citrate crystal form A.

Embodiment 2

[0060] In a 1000ml reaction bottle, add 30 grams of edenafil citrate and 630ml of distilled water, start stirring, heat up to reflux, filter while it is hot after 15 minutes, the filtrate is lowered to 38°C-42°C, keep stirring for 80 minutes, Naturally cool down to room temperature, continue stirring at 21°C-25°C for 14 hours, precipitate crystals, filter, and place in the room for 5.5 hours, then move to a vacuum drying oven, and vacuum dry for 6.5 hours to obtain the above crystalline form of aldenamorph citrate A 24.3g, the refining rate is 81%, and the content is 99.92% measured by HPLC area normalization method. After testing, it showed the characteristics of Aldenafil Citrate Form A.

Embodiment 3

[0062] Granules Containing Aldenafil Citrate Form A

[0063] Prescription: 50 grams of Aldenafil Citrate Form A, 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.

[0064] Process: PEG-4000 and aldenafil citrate crystal form A 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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PUM

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Abstract

The invention relates to 1-[3-(6, 7-dihydro-1-methyl-7-oxo-3-propyl-1H-pyrazol parallel [4, 3-d] pyridine-5-thyl)-4-ethoxybenzene sulfonyl]-cis-3, 5-lupetazin citrate or citric acid alidenafil crystalform A and preparation method thereof and also relates to drug combination containing citric acid alidenafil crystal form A and application thereof in preparation of drug for treating erection disturbance. Citric acid alidenafil raw material is dissolved with distilled water in certain proportion, stirring is carried out for 60-80 minutes while temperature is maintained to be 38-42 DEG C, and stirring is carried out for 10-15 hours while temperature is maintained to be 20-26 DEG C, 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 A is obtained, the crystal form A 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)- The new crystal form A of 4-ethoxybenzenesulfonyl]-cis-3,5-dimethylpiperazine citrate (Aildenafil citrate), its preparation method, containing The pharmaceutical composition of the crystal form A obtained in the present invention and the application of the crystal form A in the manufacture of a medicament 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 expecte...

Claims

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Application Information

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IPC IPC(8): C07D487/04A61K31/519A61P15/10
Inventor 刘桂坤
Owner 刘桂坤
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