Tianjin University

Hainan Lingkang Pharmaceutical Co., Ltd

Nantong Licheng Biological Engineering Co. Ltd

Nankai University

Zhejiang Huakang Pharmaceutical Co., Ltd.

Shenzhen Salubris Pharmaceuticals Co. Ltd.

Accendatech Co. Ltd.

Baohong Hou

Junbo Gong

Qiuxiang Yin

Ying Bao

Jingkang Wang

Chuang Xie

Linggang Tao

Hongxun Hao

Jun Lv

Qinqing Gu

Shichao Du

Kaifei Zhao

Yongli Wang

Mian Li

Yue Chen

Qiang Wu

Wulong Yang

Long Li

Duanming Tan

Qi Wang

Jiangbo Li

Yi Sun

Feng Zhang

Chuanjiang Qiu

Xiaohua Wu

Fang He

Feng Jin

Ting Zhang

Yinghui Chai

Peihua Liang

Pei Zhao

Mingshuo Chen

Lina Zhou

Jie Qi

Guiyan Wang

Zhonghua Li

Songgu Wu

Xinghua Zhu

Mingxuan Li

Jiahui Li

Shiping Tang

Mingyang Chen

Xiaopeng Song

Xin Pan

Liting Liao

Haiyan Xi

Ziyuan Di

Zhongshi Liu

Zhihong Sun

A hydrate of dimethylaminomicheliolide fumarate has a crystal form D, is high in crystallinity, smooth in particle surface, free of coalescence, high in bulk density and good in flowability, and has good stability and good reproducibility. Its preparation method includes: under a stirring action, adding dimethylamine micheliolide and fumaric acid into a mixed solvent system having a constant temperature of 30° C.-70° C. for reaction crystallization; and filtering after the reaction is finished, and drying filtered solid at normal pressure to obtain the crystal form D of the dimethylaminomicheliolide fumarate.

Hydrate of dimethylaminomicheliolide fumarate and preparation method therefor and use thereof

The present disclosure provides a technology field of caking of crystal particles, and in particular relates to a method for predicting a critical caking cycle of crystal particle. The method includes: establishing a CHS crystal bridge growth model database of a crystal particle with a same type of crystal particle to be predicted firstly, selecting existed data in the corresponding CHS crystal bridge growth model database based on an equivalent particle radius, a stored ambient temperature, and an environmental high and low humidity cycle condition of the crystal particle to be predicted, respectively, and calculating the critical caking cycle according to experience calculation equations, wherein a result obtained by calculation is a predicted critical caking cycle of the crystal particle to be predicted. The present disclosure has characteristics of time-saving, convenience, good universality, and high prediction accuracy, which can quickly predict the critical caking cycle of multi-particle crystal particle products under different humidity storage conditions within a week, resulting in greatly reducing time costs and providing guidance for storage of industrial crystal particle products.

Methods for predicting critical caking cycle of crystal particle

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 method for preparing a new crystalline form of &#x3b3;-aminobutyric acid, including the steps of: S1: preparing a &#x3b3;-aminobutyric acid solution at an initial concentration of 0.5-1.0 g/mL by adding crude &#x3b3;-aminobutyric acid to water; adding an additive to the &#x3b3;-aminobutyric acid solution, raising the temperature to 50-80&#xb0; C., stirring to produce a clear solution; and S2: obtaining a suspension by evaporating water from the product of S1 under reduced pressure and at 50-80&#xb0; C.; obtaining a wet product by filtering the suspension; drying the wet product to obtain the new crystalline form of &#x3b3;-aminobutyric acid. The preparation method of the new crystalline form of &#x3b3;-aminobutyric acid is simple, easy to operate, low in energy consumption, economical and environmentally friendly. It is suitable for large-scale industrial production.

Crystalline form of gamma-aminobutyric acid and preparation method thereof

The present invention discloses a &#x3b3;-aminobutyric acid hemihydrate crystal, its molecular formula is CHNO.0.5HO. It also discloses a method of preparing a &#x3b3;-aminobutyric acid hemihydrate crystal, including first adding crude &#x3b3;-aminobutyric acid to water to prepare a &#x3b3;-aminobutyric acid suspension at an initial concentration of 1.2-2.0 g/mL; then stirring the suspension at a constant temperature of 5-10&#xb0; C. for 6-12 hours, followed by filtering and drying to obtain the &#x3b3;-aminobutyric acid hemihydrate crystal. The &#x3b3;-aminobutyric acid hemihydrate crystal is stable, does not easily absorb moisture and agglomerate, and is convenient for further processing and use. The crystal has a large main particle size, uniform particle size distribution, high bulk density, good flowability, and a purity of &#x2265;99%. The preparation method of the crystal according to the present invention is simple, easy to operate, highly efficient and low in energy consumption, and is suitable for large-scale industrial production.

Gamma-aminobutyric acid hemihydrate crystal 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

It discloses Omeprazole Sodium semihydrate and preparation method thereof, wherein every mole of Omeprazole Sodium semihydrate contains 0.5 mole of water, and it has an X-ray diffraction pattern comprising characteristic peaks at diffraction angles 2&#x3b8; of 6.26&#xb0;&#xb1;0.1&#xb0;, 11.10&#xb0;&#xb1;0.1&#xb0;, 12.20&#xb0;&#xb1;0.1&#xb0;, 15.58&#xb0;&#xb1;0.1&#xb0;, 16.02&#xb0;&#xb1;0.1&#xb0;, 17.12&#xb0;&#xb1;0.1&#xb0;, 19.08&#xb0;&#xb1;0.1&#xb0;, 21.00&#xb0;&#xb1;0.1&#xb0;, 22.68&#xb0;&#xb1;0.1&#xb0;, 23.48&#xb0;&#xb1;0.1&#xb0;, 24.08&#xb0;&#xb1;0.1&#xb0;, 26.52&#xb0;&#xb1;0.1&#xb0; and 28.08&#xb0;&#xb1;0.1&#xb0;. A raw material of Omeprazole Sodium hydrate is added into an organic solvent, stirring for 2&#x2dc;9 hours at constant temperature of 25&#x2dc;60&#xb0; C., thereafter Omeprazole Sodium semihydrate is provided after filtrating and drying.

Omeprazole Sodium semihydrate and preparation method thereof

This invention provides a new preparation method of Clopidogrel Hydrogen Sulfate spherical crystal form I, using single 2-butanol as solvent, controlling the concentration, addition way and addition speed of sulfuric acid used to salify to shorten the process time, thus separating out Clopidogrel Hydrogen Sulfate from solution system stably with spherality. And the Clopidogrel Hydrogen Sulfate obtained complies with the requirements of the follow-up process on residual solvent, bulk density and mobility.

Method for preparing spherical Clopidogrel Hydrogen Sulfate polymorph I

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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Tianjin, China

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