07-12-2017 дата публикации
Номер: US20170349609A1
Автор:
Hongxun Hao,
Linggang Tao,
Fang He,
Baohong Hou,
Jingkang Wang,
Jun Lv,
Qiuxiang Yin,
Yongli Wang,
Junbo Gong,
Chuang Xie,
Ying Bao
A novel crystalline form is defined by diffraction angle 2θ° of X-ray powder diffraction pattern and characteristic peak of differential scanning calorimetry (DSC). The novel crystalline form of Cefamandole Nafate is prepared as follows: adding Cefamandole Nafate in solid state to an organic solvent to form a suspension with a concentration of 0.04˜0.3 g/ml, stirring the suspension at 40˜50° C. for a period of time, and then cooling to 5˜15° C. at certain cooling rate, continuing to stir for a period of time, then suction filtrating the obtained suspension, the resulting filer cake is Cefamandole Nafate as wet product, which is dried to constant weight to provide the novel crystalline form of Cefamandole Nafate as final product. 1. (canceled)2. (canceled)3. A method for preparing a crystalline form of Cefamandole Nafate having an X-ray powder diffraction pattern having characteristic peaks expressed in degrees 2θ at 4.0±0.2 , 4.7±0.2 , 6.2±0.2 , 7.5±0.2 , 9.9±0.2 , 10.8±0.2 , 14.5±0.2 , 15.8±0.2 , 16.3±0.2 , 17.4±0.2 , 18.1±0.2 , 19.2±0.2 , 20.1±0.2 , 21.4±0.2 , 22.2±0.2 , 22.8±0.2 , 23.9±0.2 , 24.9±0.2 , 30.1±0.2 , and 34.1±0.2 and a differential scanning calorimetry thermogram (DSC) having an endothermic peak at 165±2° C. , characterized in that: adding Cefamandole Nafate in solid state to an organic solvent to form a suspension with a concentration of 0.04˜0.3 g/ml , stirring the suspension at 40˜50° C. , then cooling to 5˜15° C. and stirring , and suction filtrating the obtained suspension , the resulting filer cake is Cefamandole Nafate as wet product , which is dried to constant weight to provide the crystalline form of Cefamandole Nafate.4. The method according to claim 3 , characterized in that claim 3 , said organic solvent is selected from one of methanol claim 3 , ethanol claim 3 , n-propanol claim 3 , isopropanol claim 3 , n-butanol claim 3 , isobutanol claim 3 , sec-butanol claim 3 , iso-pentanol claim 3 , n-pentanol claim 3 , ethyl acetate claim 3 , 1 ...
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