公开(公告)号：US20210300892A1

公开(公告)日：2021-09-30

申请号：US17208043

申请日：2021-03-22

申请人： Tianjin University

发明人： Ying BAO ,  Feng ZHANG ,  Peihua LIANG ,  Baohong HOU ,  Chuang XIE ,  Ting ZHANG ,  Yinghui CHAI

IPC分类号： C07D401/04

摘要： The disclosure relates to etoricoxib solvates and a preparation method thereof. A solvent is a hydrogen bond donor solvent with a polarity value π* ranging from 60 to 100 or a hydrogen bond acceptor solvent with a polarity value π* ranging from 92 to 100. Solvents with a polarity value π* within the above range all can form corresponding etoricoxib solvates with etoricoxib. The etoricoxib solvate can be prepared by cooling crystallization or suspension crystallization. A 1,2-propanediol solvate of etoricoxib and a dimethyl sulfoxide (DMSO) solvate of etoricoxib provided in the present disclosure have high thermal stability, unique crystal form, large size, concentrated distribution, and prominent flowability and is safe, pharmaceutically acceptable, and not easy to agglomerate. Compared with etoricoxib, the etoricoxib solvates exhibit significantly improved solubility. Moreover, preparation of the solvates requires low consumption in time, energy, and solvent, and has high efficiency, with a molar yield higher than 90%.

公开(公告)号：US20170044184A1

公开(公告)日：2017-02-16

申请号：US15304824

申请日：2015-11-20

申请人： TIANJIN UNIVERSITY ,  HAINAN LINGKANG PHARMACEUTICAL CO., LTD

发明人： Hongxun HAO ,  Linggang TAO ,  Zhihong SUN ,  Baohong HOU ,  Jun LV ,  Qiuxiang YIN ,  Yongli WANG ,  Junbo GONG ,  Chuang XIE ,  Ying BAO

IPC分类号： C07D501/60

CPC分类号： C07D501/60 ,  C07B2200/13 ,  C07D501/12 ,  C07D501/28

摘要： A novel crystalline form of Cefathiamidine compound and its preparation method, characterizing in its X-ray powder diffraction pattern and differential scanning calorimetry thermogram. Dissolving Cefathiamidine compound with a purity of 98% or higher in a solvent at a temperature of 30˜45° C. to form a solution, whose concentration is controlled within 0.05˜0.2 g/mL, and then adding a solventing-out agent to the solution, wherein the amount of the solventing-out agent is 3˜5 times (in volume) of that of the solvent; followed by cooling the solution down to 0˜10° C. at a rate of 0.2˜1° C./min; continuing to stir for 1˜3 hours, and separating the obtained solid-liquid suspension to provide a novel crystalline form of Cefathiamidine compound after drying.

摘要翻译： 尖晶石化合物的新型结晶形式及其制备方法，其X射线粉末衍射图和差示扫描量热法热分析图表征。 在溶剂中在30〜45℃的温度下溶解纯度为98％以上的头孢硫脒化合物，形成浓度为0.05〜0.2g / mL的溶液，然后加入溶剂 溶剂，其中溶剂量为溶剂量的3〜5倍（体积）; 然后以0.2〜1℃/分钟的速度将溶液冷却至0〜10℃; 继续搅拌1〜3小时，分离得到的固液悬浮液，干燥后提供新型的头孢噻肟化合物结晶形式。

公开(公告)号：US20170197937A1

公开(公告)日：2017-07-13

申请号：US15304861

申请日：2015-11-20

申请人： TIANJIN UNIVERSITY ,  HAINAN LINGKANG PHARMACEUTICAL CO., LTD

发明人： Hongxun HAO ,  Linggang TAO ,  Shen JIANG ,  Yongli WANG ,  Jingkang WANG ,  Jun LV ,  Qiuxiang YIN ,  Baohong HOU ,  Zhao XU ,  Chuang XIE ,  Zhao WANG

IPC分类号： C07D401/12

CPC分类号： C07D401/12 ,  A61K9/0019 ,  A61K31/4439 ,  C07B2200/13

摘要： A novel crystalline form is defined by using diffraction angle 2θ° of X-ray powder diffraction pattern and characteristic peaks of differential scanning calorimetry (DSC). Pantoprazole Sodium solid is added to an alcohol solvent to form a suspension with a concentration of 0.05˜0.2 g/mL, and then an antioxidant is added to the suspension, completely dissolving the solid at a temperature of 15˜35° C., and a solventing-out agent is dropwise added to the solution under the application of ultrasonic wave, wherein the amount of the solventing-out agent is 3˜10 times (in volume) of the alcohol solvent; followed by cooling the solution down to 0˜5° C., continuing to stir for 1˜3 h, and suction filtrating obtained solid-liquid suspension to provide a novel crystalline form of Pantoprazole Sodium crystal after drying the product to constant weight.

公开(公告)号：US20170050982A1

公开(公告)日：2017-02-23

申请号：US15305661

申请日：2015-11-20

申请人： TIANJIN UNIVERSITY ,  HAINAN LINGKANG PHARMACEUTICAL CO., LTD

发明人： Hongxun HAO ,  Linggang TAO ,  Fang He ,  Baohong HOU ,  Jingkang WANG ,  Jun LV ,  Qiuxiang YIN ,  Yongli WANG ,  Junbo GONG ,  Chuang XIE ,  Ying Bao

IPC分类号： C07D501/36 ,  C07D501/12

CPC分类号： C07D501/36 ,  C07B2200/13 ,  C07D501/12

摘要： 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.

摘要翻译： 新型结晶形式由X射线粉末衍射图的衍射角2θ°和差示扫描量热法（DSC）的特征峰定义。 头孢丹多奈非糖酸盐的新型结晶形式如下制备：将固体状态的头孢马替奈啡钠加入到有机溶剂中，形成浓度为0.04〜0.3g / ml的悬浮液，在40〜50℃下搅拌悬浮液一段时间 的时间，然后以一定的冷却速度冷却至5〜15℃，继续搅拌一段时间，然后抽滤所得悬浮液，得到的滤饼为头孢丹多，作为湿产品干燥至恒定 重量，以提供新颖的头孢曼陀螺Nafate的结晶形式作为最终产品。