发明名称 METHOD FOR ISOLATING PHARMACEUTICALLY EXPLOITABLE ETIDRONATE DISODIUM SALT
摘要 1. A method for isolating etidronate disodium, characterized in that a) a liquid-liquid dispersion, consisting of - an aqueous-organic and - an aqueous phase comprising the etidronate disodium salt is adjusted to a temperature of 0 degree C to 30 degree C and intensively stirred, b) then a coarse grain fraction is precipitated from the liquid-liquid dispersion, c) in a second, delayed step a fine grain fraction is precipitated from the organic phase. 2. The method as claimed in claim 1, characterized in that the liquid-liquid dispersion has a total water content of 25 to 35% by volume. 3. The method as claimed in claim 1 or 2, characterized in that the liquid-liquid dispersion has a total etidronate disodium salt content of 10 to 100 g/kg of dispersion. 4. The process as claimed in one of claims 1 to 3, characterized in that d) the fine grain fraction is separated from the coarse grain fraction by classification and fed back into the method. 5. The method as claimed in claim 4, characterized in that e) the coarse grain fraction according to step d) is filtered and dried by means of drying in a moving bed up to a final temperature of 85 degree C to 100 degree C. 6. The method as claimed in one of claims 1 to 5, characterized in that the liquid-liquid dispersion is preferably adjusted to between 5 degree C and 10 degree C. 7. The method as claimed in one of claims 1 to 6, characterized in that the aqueous-organic phase is an isopropanol/water phase. 8. The method as claimed in one of claims 1 to 7, characterized in that, for the liquid-liquid dispersion, an aqueous solution of etidronate disodium is added to a solvent consisting of isopropanol/water. 9. Etidronate disodium, obtainable by the method as claimed in one of claims 1 to 8. 10. Etidronate disodium, whose solid form is characterized by an X-ray powder diffractogram according to figure 1. 11. Etidronate disodium, whose solid form is characterised by an IR spectrum according to figure 2.
申请公布号 EA004688(B1) 申请公布日期 2004.06.24
申请号 EA20030000396 申请日期 2001.09.28
申请人 SCHERING AKTIENGESELLSCHAFT 发明人 GRAWE, DETLEF;SCHMIDT, BARBARA;RATHE, HARALD
分类号 C07F9/38;(IPC1-7):C07F9/38 主分类号 C07F9/38
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