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High-purity ozagrel compound

A high-purity compound technology, applied in the field of medicine, can solve the problems of low purity of sodium ozagrel, high cost, unsatisfactory foreign matter, etc., and achieve the effects of being suitable for large-scale industrial production, easy to operate, and simple in method

Inactive Publication Date: 2012-01-11
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The synthetic method has high cost and low yield, and the prepared ozagrel sodium has lower purity
[0008] Ozagrel raw materials are produced by many manufacturers in China, but their quality is directly related to the quality of the preparations produced. For example, in the process of producing ozagrel sodium powder injections with poor quality, foreign matter can be seen. If the requirements are met, there will be phenomena such as blue dots and color blocks, which will affect the production yield and increase the cost

Method used

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  • High-purity ozagrel compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The refining of embodiment 1 ozagrel

[0021] 100g of crude ozagrel was added into 2000ml of water to form an aqueous dispersion, and then 0.1mol / L sodium hydroxide solution was added dropwise to the aqueous dispersion until clarified to obtain a clear solution, and 23g of activated carbon was added to the resulting clear solution for adsorption for 20 minutes. Filtrate decarburization, add 0.5 mol / L hydrochloric acid solution to the obtained filtrate to adjust the pH to 1.0, precipitate a solid, filter, wash with 50ml×3 water, and dry under reduced pressure at 50°C for 8 hours to obtain high-purity ozagrel 92.6 g, the yield is 92.6%, and the purity detected by HPLC is 99.94%.

Embodiment 2

[0022] The refining of embodiment 2 ozagrel

[0023] Add 100 g of crude ozagrel into 2000 ml of water to form an aqueous dispersion, then add dropwise 0.5 mol / L sodium hydroxide solution to the aqueous dispersion until clarification, to obtain a clear solution, add 1.15 g of activated carbon to the resulting clear solution for adsorption for 30 min, Filtrate decarburization, add 1 mol / L nitric acid solution to the obtained filtrate to adjust the pH value to 3.0, precipitate a solid, filter, wash with 50ml×3 water, and dry under reduced pressure at 60°C for 5 hours to obtain 93.1g of high-purity ozagrel , the yield was 93.1%, and the purity detected by HPLC was 99.92%.

Embodiment 3

[0024] The refining of embodiment 3 ozagrel

[0025] Add 100 g of crude ozagrel into 2000 ml of water to form an aqueous dispersion, then add dropwise 0.2 mol / L sodium hydroxide solution to the aqueous dispersion until clarification, to obtain a clear solution, add 2.3 g of activated carbon to the resulting clear solution for adsorption for 30 min, Filtrate decarburization, add 5 mol / L phosphoric acid solution to the obtained filtrate to adjust the pH value to 2.0, precipitate a solid, filter, wash with water 50ml×3, and dry under reduced pressure at 55°C for 6 hours to obtain 94.5g of high-purity ozagrel , the yield was 94.5%, and the purity detected by HPLC was 99.96%.

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Abstract

The invention relates to a high-purity ozagrel compound, and a preparation method of the ozagrel compound guarantees the quality of raw materials, and avoids the phenomenon that visible foreign matters are unqualified in the production process. The preparation method includes the following steps: (1) adding crude ozagrel in water to form aqueous dispersion; (2) then dropwise adding sodium hydroxide solution in the aqueous dispersion until the aqueous dispersion is clear to obtain clear solution; and (3) adding activated carbon in the clear solution for adsorption, conducting filtering and decarburization, adding acid in obtained filtrate to adjust pH value, precipitating solids, filtering, washing, and drying to obtain the high-purity ozagrel.

Description

technical field [0001] The invention relates to a method for preparing an ozagrel compound, which belongs to the technical field of medicine. Background technique [0002] Ozagrel (English name: ozagrel), its chemical name is: trans-3-[4-(1H-imidazolyl-1-methyl)phenyl]-2-acrylic acid, molecular formula: C 13 h 12 N 2 o 2 , molecular weight: 228.25, structural formula: [0003] [0004] Ozagrel is a highly effective and selective inhibitor of thromboxane synthase, which inhibits the synthesis of thromboxane A2 (TXA2) and promotes the production of prostacyclin (PGI2), thereby anti-platelet aggregation, reducing blood viscosity, and promoting thrombosis Decomposition and dilation of blood vessels and other effects. Therefore, it is especially suitable for inhibiting cerebral vasospasm, increasing cerebral blood flow, improving microcirculation disorders and abnormal energy metabolism in the brain, and improving cerebral ischemic symptoms and cerebral thrombosis (acute ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/56
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD
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