Tianjin University

Hainan Lingkang Pharmaceutical Co., Ltd

Chuang Xie

Baohong Hou

Ying Bao

Linggang Tao

Junbo Gong

Qiuxiang Yin

Hongxun Hao

Jun Lv

Yongli Wang

Jingkang Wang

Fang He

Ting Zhang

Feng Zhang

Pei Zhao

Mingshuo Chen

Lina Zhou

Zhihong Sun

Yinghui Chai

Peihua Liang

A crystalline form of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide, with a large particle size, which belongs to a triclinic crystal system and space group P-1. A crystallization method for making the crystalline form of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide, comprising adding a solid of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide to a solvent and mixing; followed by heating to 50 to 70&#xb0; C. to achieve complete dissolution; cooling the solution to room temperature; and adding an anti-solvent to the resulting solution to cause precipitation of crystals. The crystals are allowed to grow at a constant temperature for 10 to 60 minutes, so as to give a slurry containing the crystals. Said slurry is subjected to filtration and then drying to obtain the crystalline form of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide.

Crystalline form of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide with large particle size and crystallization method for making same

The disclosure relates to etoricoxib solvates and a preparation method thereof. A solvent is a hydrogen bond donor solvent with a polarity value &#x3c0;* ranging from 60 to 100 or a hydrogen bond acceptor solvent with a polarity value &#x3c0;* ranging from 92 to 100. Solvents with a polarity value &#x3c0;* 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%.

Etoricoxib solvates and preparation method thereof

A novel crystalline form is defined by diffraction angle 2&#x3b8;&#xb0; 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&#x2dc;0.3 g/ml, stirring the suspension at 40&#x2dc;50&#xb0; C. for a period of time, and then cooling to 5&#x2dc;15&#xb0; 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.

Crystalline form of cefamandole nafate compound, preparation and preparing method thereof

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&#x2dc;45&#xb0; C. to form a solution, whose concentration is controlled within 0.05&#x2dc;0.2 g/mL, and then adding a solventing-out agent to the solution, wherein the amount of the solventing-out agent is 3&#x2dc;5 times (in volume) of that of the solvent; followed by cooling the solution down to 0&#x2dc;10&#xb0; C. at a rate of 0.2&#x2dc;1&#xb0; C./min; continuing to stir for 1&#x2dc;3 hours, and separating the obtained solid-liquid suspension to provide a novel crystalline form of Cefathiamidine compound after drying.

Crystal form of Cefathiamidine compound and preparation method therefor

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Chuang Xie