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

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

Inactive Publication Date: 2012-07-25
刘桂坤
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
Comparison scheme
Effect test

Embodiment 1

[0094] In a 100ml reaction flask, add 3 grams of aldenafil citrate, 85ml of distilled water / absolute ethanol (50:50, volume ratio), start stirring, heat and heat up to reflux temperature, filter while hot after 15 minutes, seal the container Put the filtrate in a filter bottle, place it indoors, cool down naturally, drop to 30°C-35°C, keep it at a temperature for 58 hours, precipitate out crystals, filter, place indoors for 1 hour, and dry to obtain citrate aldenafil crystalline form D 1.8g, its melting point is m.p 201.9-203.1°C, the purification 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 , are the three-dimensional structure projection diagram, unit cell projection diagram, infrared spectrum and X-ray powder diffraction diagram of aldenafil citrate crystalline form D, showing the characteristics of citrate aldenafil crystalline form D.

Embodiment 2

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

Embodiment 3

[0098] Granules containing edenafil citrate form D

[0099] Prescription: 50 grams of edinafil citrate form D, 650 grams of lactose, 100 grams of crospovidin, 90 grams of PEG-400000, 135 grams of hydroxypropyl methylcellulose, appropriate amount of distilled water, made into 1000 bags.

[0100] Process: PEG-4000 and citrate adenafil crystal form D are crushed together, passed through an 80-mesh sieve, mixed with other materials to make 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-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 preparation method thereof, containing the present invention The obtained pharmaceutical composition of the crystal form D and the use of the crystal form D in the manufacture of a medicament for treating male erectile dysfunction (ED). Background technique [0002] Male erectile dysfunction (ED) is a common disease, which can be defined as inability to erect the penis, inability to ejaculate, or both. 65% of men. There are about 125 million men worldwide with erectile dysfunction of varying degrees, and it is expected to reach 322 million by 2025 (Moreland RB, et al, J Pharmacol Exp Ther, 2001, 296(2): 225-234.). Therefore, research and development of safe and effective new drugs or new drug delivery systems for ED have important clinical va...

Claims

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Application Information

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