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

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Problems solved by technology

Chinese patent (application number 02100198.7) discloses edenafil and its preparation me

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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