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Aildenafil citrate crystal form C and preparation method and application thereof

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

Inactive Publication Date: 2010-04-07
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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  • Aildenafil citrate crystal form C and preparation method and application thereof
  • Aildenafil citrate crystal form C and preparation method and application thereof
  • Aildenafil citrate crystal form C and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] In a 1000ml reaction bottle, add 20 grams of edenafil citrate, 440ml of distilled water / acetone mixture (4.5:5.5, volume ratio), start stirring, heat up to reflux temperature, and filter while hot after 15 minutes. The filtrate was lowered to 28°C-32°C, kept warm and stirred for 45 minutes; then cooled naturally to 23±3°C, continued to stir for 10 hours, precipitated crystals, filtered, and placed in the room for 2 hours, then moved to a vacuum oven and dried in vacuum (0.08 -0.10Mpa) for 4 hours, 17.6 g of the above crystalline form C of edenamorph citrate was obtained, and the refining rate was 88%. Adopt HPLC area normalization method to measure content 99.90%, see Figure 1-Figure 3 , detected by X-ray diffractometer, infrared spectrometer and thermal analyzer, showing the characteristics of Aldenamorph Citrate Form C.

Embodiment 2

[0060] In a 2000ml reaction bottle, add 35 grams of edenafil citrate, 630ml of distilled water / acetone (6:4, volume ratio), start stirring, heat up to reflux, and filter while hot after 18 minutes. The filtrate was lowered to 30°C-32°C, kept warm and stirred for 30 minutes; then cooled naturally to 23±3°C, continued to stir for 8 hours, precipitated crystals, filtered, and placed in the room for 3 hours, then moved to a vacuum oven and dried in vacuum (0.08 -0.10Mpa) for 5 hours, 31.9 g of the above-mentioned edenamorph citrate crystal form C was obtained, and the purification rate was 91.1%. The content measured by the HPLC area normalization method is 99.90%, and after testing, it shows the characteristics of Aldenamorph citrate crystal form C.

Embodiment 3

[0062] Granules Containing Aldenafil Citrate Form C

[0063] Prescription: 50 grams of Aldenafil Citrate Form C, 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 C 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-pyrazolo [4,3-d] pyrimidine-5-yl)-4-ethoxybenzenesulfonyl]-cis-3,5-dimethyl-piperazine citrate or a aildenafil citrate crystal form C and a preparation method thereof. The invention also relates to a medicinal composition containing the aildenafil citrate crystal form C and application thereof in preparing medicaments for treating male erection disturbance. An unprecedented aildenafil citrate crystal form C is proved to be obtained through the steps of dissolving an aildenafil citrate raw material in a mixed solution of distilled water and acetone at a certain proportion, keeping the temperature for 8 to 10 hours at a certain temperature while stirring, and testing the prepared product by an X-ray powder diffractometer, a thermogravimetric analyzer and an infrared spectrometer; and the crystal form C can form a composition together with one or more pharmaceutically acceptable carriers, an excipient or a diluent, and can be effectively applied to the treatment of 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)- New crystal form C of 4-ethoxybenzenesulfonyl]-cis-3,5-dimethylpiperazine citrate (Aildenafil citrate) and its preparation method, containing the present The pharmaceutical composition of the obtained crystal form C and the application of the new crystal form C 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 expect...

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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