Method for preparing ozagrel sodium crystal

A crystallization technology of ozagrel sodium, which is applied in the crystallization process field of medicinal compound ozagrel sodium, can solve the problems of low yield, high content of "related substances", lack of fine filtration, crystal growth, etc., and achieve high yield High, low content of related substances, high purity effect

Active Publication Date: 2009-04-01
HAINAN BIKAI PHARM CO LTD
0 Cites 14 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0003] In the existing ozagrel preparation method, the crystallization process during refining is only to dissolve the crude ozagrel and then filter and cool i...
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Abstract

The invention relates to a simple technical process used for preparing high-pure ozagrel sodium crystal. The process basically includes the following steps: the raw ozagrel sodium is added into ethanol and then heated for dissolving; active carbon is added for decoloring and filtering is carried out under the heated condition; the filtrate is filtered in a refined way by a microfiltration membrane, collected, heated first and then cooled slowerly; and the temperature is controlled to be 25 DEG C to 60 DEG C for temperature-preservation crystallization and then the temperature is reduced slowly and cooled for crystallization; finally the crystal is collected. The crystal prepared by the method is high in purity and yielding and low in impurity content; therefore the therapy effect of the product is effectively enhanced and the cost is reduced simultaneously.

Application Domain

Organic chemistryCardiovascular disorder

Technology Topic

Sodium ozagrelActive carbon +9

Examples

  • Experimental program(5)

Example Embodiment

[0009] Example 1
[0010] Add the crude ozagrel sodium solution to 99% ethanol, heat to 80°C to dissolve it, add activated carbon to decolorize for 30 minutes, filter while hot, continue the filtrate through a 0.45 micron membrane, collect the filtrate, and then continue the filtrate Raise the temperature to 80°C, slowly decrease the temperature to about 45°C, control the temperature at 40-43°C and keep the crystals for 2.5 hours, then continue to cool to 4-10°C for 2 hours, then slowly lower the temperature, cool and crystallize, finally collect the crystals, and collect Rate: 90.8%, content: 100.3%.

Example Embodiment

[0011] Example 2
[0012] Add the crude ozagrel sodium solution to 80% ethanol, heat to 80°C to dissolve it, add activated carbon to decolorize for 30 minutes, filter while hot, continue the filtrate through a 0.45 micron membrane, collect the filtrate, and then continue the filtrate Raise the temperature to 80°C, slowly lower the temperature to about 45°C, control the temperature at 30-45°C to keep the crystals for 2.5 hours, then continue to cool down to 4-10°C for 2 hours, then slowly lower the temperature, cool and crystallize, finally collect the crystals, and collect Rate: 90.9%, content: 100.1%.

Example Embodiment

[0013] Example 3
[0014] Add the crude ozagrel sodium solution to 95% ethanol, heat to 60℃ to dissolve it, add activated carbon to decolorize for 30 minutes, filter while hot, continue the filtrate through a 0.45 micron membrane, collect the filtrate, and then continue the filtrate Raise the temperature to 60°C, slowly decrease the temperature to about 45°C, control the temperature at 40-43°C and keep the crystals for 2.5 hours, then continue to cool to 4-10°C for 2 hours, then slowly lower the temperature, cool down and crystallize, and finally collect the crystals. Rate: 91.3%, content: 99.9%.

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Description & Claims & Application Information

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