Type I clopidogrel hydrogen sulfate salt preparation method
The invention discloses a type I clopidogrel hydrogen sulfate salt preparation method which comprises the following steps: (1) mixing clopidogrel salt with an organic solvent, adding water, adding an acid binding agent or an acid binding agent water solution to the solvent, stirring for reaction to...
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Zusammenfassung: | The invention discloses a type I clopidogrel hydrogen sulfate salt preparation method which comprises the following steps: (1) mixing clopidogrel salt with an organic solvent, adding water, adding an acid binding agent or an acid binding agent water solution to the solvent, stirring for reaction to generate clopidogrel free alkali, standing for layering, extracting aqueous phase with the same organic solvent, combining the organic phase, washing with water, recovering the solvent to dry; and (2) adding an organic solvent into the concentrated clopidogrel free alkali, stirring to fully dissolve the clopidogrel free alkali, cooling, adding seed crystal, according to the molar ratio of sulfuric acid to clopidogrel free alkali of 0.9-1.05:1, dropwise adding sulfuric acid solution into the solution, standing, filtering, and drying to obtain the type I clopidogrel hydrogen sulfate. The type I clopidogrel hydrogen sulfate obtained by the method has the advantages of high purity and stable property. |
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