Hainan Lingkang Pharmaceutical Co., Ltd

Tianjin University

Linggang Tao

Baohong Hou

Ying Bao

Jun Lv

Hongxun Hao

Junbo Gong

Qiuxiang Yin

Chuang Xie

Yongli Wang

Jingkang Wang

Long Li

Fang He

Zhihong Sun

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

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

A method for treating cefotiam hydrochloride, comprises the following steps: step 1), dissolving the raw material cefotiam hydrochloride in water, treating it with an acidic salt, then cooling it, and filtering the precipitate to obtain an aqueous filtrate; step 2), adding a water-immiscible solvent to the above aqueous solution for extraction, and then separating the organic phase containing impurities to obtain an aqueous solution containing cefotiam hydrochloride; step 3) adding to the aqueous solution a poor solvent of cefotiam hydrochloride and controlling the temperature for recrystallization, washing the educed crystals by centrifugation, and drying them to obtain purified cefotiam hydrochloride. The cefotiam content of the refined cefotiam hydrochloride obtained by the method of the present invention is not less than 86%, the content of polymeric impurities is less than 0.3%, and the content of insoluble microparticles in the injection prepared therefrom is quite low.

Process for purifying cefotiam hydrochloride

A process for preparing a pure alanylglutamine comprises the steps of: 1) reacting N-(&#x3b1;-chloro)-propionyl-glutamine and hydrazine compound to obtain an alanylglutamine crude product; 2) mixing anhydrous methanol and the alanylglutamine crude product to provide a filter cake; 3) dissolving the filter cake in water, heating, adding ethanol, and cooling to yield the pure alanylglutamine.

Alanyl glutamine compound and preparation method thereof

It discloses a process for refining Aztreonam, comprising the steps of 1) treating Aztreonam material with an alkali metal alkoxylate or an alkali earth metal alkoxylate under heating in the presence of a suitable solvent or a mixture of solvents, followed by adjusting the pH value with a suitable acid and cooling down to precipitate Aztreonam, which provides a primary purified Aztreonam; 2) adsorbing Aztreonam with strongly basic ion exchange resin, followed by eluting the resin and collecting the eluate, to provide a secondary purified Aztreonam after concentration under reduced pressure; 3) adjusting the pH value with a suitable acid to allow crystallization, followed by centrifuging and washing the resultant crystals, to provide a tertiary purified Aztreonam after drying. The refined Aztreonam product has a purity of no less than 99.2%, mostly no less than 99.5%, with little residue on ignition and significantly low content of heavy metals.

Purification method of aztreonam

A process for purifying lansoprazole comprises 1) loading crude lansoprazole material onto a macroporous resin column; 2) concentrating the eluate from the column in a crystallization vessel by vacuum; 3) seeding lansoprazole crystal; 4) crystallizing the lansoprazole; 5) separating the precipitated crystals. The process especially has large processing capacity, can be carried out continuously and therefore suitable for industrial production, improving the quality of formulated products and reducing side effects.

Lansoprazole compound and novel preparation method thereof

A novel process for purifying Cefmenoxime hydrochloride comprises: 1) adding a solvent wherein Cefmenoxime hydrochloride is insoluble at the temperature less than 30&#xb0; C., filtering after vigorous stirring, washing the filter cake with a solvent wherein Cefmenoxime hydrochloride is insoluble at a temperature less 20&#xb0; C., and drying; 2) placing the filter cake into ammonium hydroxide, controlling the pH value less than 9 with a gentle agitation to obtain Cefmenoxime acid solution in ammonium hydroxide, and then filtering out the precipitate; 3) adding hydrochloric acid at a concentration of 0.5-4 mol/L to Cefmenoxime acid solution in ammonium hydroxide slowly and controlling the temperature between 30-60&#xb0; C. and the final pH between 0.5-3.0, and then cooling down to a minimum of 10&#xb0; C. and standing still to allow crystallization, filtrating and vacuum drying.

Method for preparing cefmenoxime hydrochloride compound

A novel process for refining Ceftizoxime sodium compound, comprises the steps of: 1) dissolving crude Ceftizoxime sodium in water, and extracting with cyclohexane or ethyl acetate, followed by separating the organic phase containing impurities, producing an aqueous phase containing Ceftizoxime sodium; 2) adding ammonia or ammonium hydroxide into the above aqueous phase while stirring, followed by filtrating the precipitate, producing an aqueous filtrate containing Ceftizoxime sodium; 3) adding an alcoholic solvent in the aqueous solution and recrystallizing under controlled temperature, followed by centrifuging and washing the resultant crystals, producing the refined Ceftizoxime sodium after drying; and 4) optionally returning the mother liquid of the recrystallization process to step 3).

Method for purifying Ceftizoxime sodium

It discloses a novel process for refining cefamandole nafate, comprising: 1) adsorbing cefamandole nafate with strongly acidic ion exchange resin, followed by eluting the resin and collecting the eluate, to provide a primary purified cefamandole acid after concentration under reduced pressure; 2) neutralizing the primary purified cefamandole acid with an aqueous solution of sodium hydroxide or an aqueous solution of basic salt of sodium, followed by adjusting the pH value and filtrating out the insoluble substances with heating, thereby providing a secondary purified aqueous solution of cefamandole nafate; and 3) adding ethanol in a volume ratio between ethanol and water of 4:6 into the aqueous solution, to allow recrystallization under controlling the temperature, to provide a tertiary purified cefamandole nafate. The refined cefamandole nafate product has a purity of no less than 99.5%, mostly no less than 99.6%, with significantly low content of heavy metals.

Refining process of Cefamandole sodium

The present invention relates to a novel process for refining Cefmetazole sodium, comprising the steps of: 1) dissolving Cefmetazole sodium material in water, and extracting after adding a water-immiscible organic solvent(s), followed by separating the organic phase containing impurities, to provide an aqueous phase containing Cefmetazole sodium; 2) treating by adding an alkoxide of alkali metal or alkaline earth metal into the above aqueous phase, followed by filtrating the precipitate, to provide an aqueous filtrate; and 3) adding ethanol or acetone in the aqueous solution and recrystallizing, followed by centrifuging and washing the resultant crystals, to provide the refined and purified Cefmetazole sodium after drying. The purity of Cefmetazole sodium material can be greatly improved by the process of the present invention.

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Wuyi, China

Linggang Tao