Disclosed are a novel polymorphic cefuroxime sodium compound and a preparation method for crystals thereof, where the novel polymorphic cefuroxime sodium compound is prepared by employing a particle process crystal product molecular assembly and morphological optimization technique. Stability tests show that the present novel polymorphic compound is characterized by high purity, low impurity content, low hygroscopicity, and great stability. At the same time, also disclosed is a preparation—cefuroxime sodium for injection use—prepared by employing the cefuroxime sodium.
C07D 501/34 - Radicaux méthylène substitués par des atomes d'oxygèneLeurs lactones avec le groupe carboxyle-2 avec le radical amino-7 acylé par des acides carboxyliques contenant des hétérocycles
CEFATHIAMIDINE NOVEL CRYSTAL COMPOUND USING PARTICLE PROCESS CRYSTAL PRODUCT MOLECULAR ASSEMBLY AND MORPHOLOGY OPTIMISATION TECHNOLOGY AND FORMULATION THEREOF
Disclosed in the present invention are a cefathiamidine novel crystal compound and a crystallisation preparation method therefor, the cefathiamidine novel crystal compound being prepared using particle process crystal product molecular assembly and morphology optimisation technology. The present crystal compound has the characteristics of high purity, low impurity content, good fluidity, and good stability. Also disclosed in the present invention is a formulation prepared using said cefathiamidine: cefathiamidine for injection.
C07D 501/28 - Radicaux méthylène substitués par des atomes d'oxygèneLeurs lactones avec le groupe carboxyle-2 avec le radical amino-7 acylé par un acide carboxylique aliphatique, lequel est substitué par des hétéro-atomes
C07D 501/04 - Préparation à partir de composés contenant déjà les systèmes cycliques ou cycliques condensés, p. ex. par déshydrogénation du cycle, par introduction, élimination ou modification de substituants
A61K 31/545 - Composés contenant des systèmes cycliques thia-5 aza-1 bicyclo [4.2.0] octane, c.-à-d. composés contenant un système cyclique de formule , p. ex. céphalosporines, céfaclor, céphalexine
Disclosed are a cefmenoxime hydrochloride new crystalline compound and crystallization preparation method thereof; said cefmenoxime hydrochloride new crystalline compound is formed using particle processing for molecular assembly and morphological optimization of a crystalline product. The present compound has the features of high purity, good fluidity, and good stability. Also disclosed is a formulation -- cefmenoxime hydrochloride used for injection -- fabricated using the described cefmenoxime hydrochloride compound.
A61K 31/546 - Composés contenant des systèmes cycliques thia-5 aza-1 bicyclo [4.2.0] octane, c.-à-d. composés contenant un système cyclique de formule , p. ex. céphalosporines, céfaclor, céphalexine contenant d'autres hétérocycles, p. ex. céphalotine
Disclosed is a new industrial crystallisation technique for cefuroxime sodium, wherein a supercritical fluid extraction technique is combined with conventional crystallization techniques to realize the recrystallization of cefuroxime sodium. Within the whole crystallization system, under the conditions of a specific temperature and pressure, the processes of extraction, adsorption, crystallization and drying are done so as to realize the recrystallization of cefuroxime sodium with the combined action of a supercritical fluid, a solvent, an extraction pool and a crystallizing pool. The present method has a high separation efficiency and few impurities, and greatly improves the quality of preparation products.
C07D 501/34 - Radicaux méthylène substitués par des atomes d'oxygèneLeurs lactones avec le groupe carboxyle-2 avec le radical amino-7 acylé par des acides carboxyliques contenant des hétérocycles
A61K 9/14 - Préparations médicinales caractérisées par un aspect particulier à l'état particulaire, p. ex. poudres
5.
OMEPRAZOLE SODIUM COMPOUND PREPARED BY USING PARTICLE PROCESSING FOR MOLECULAR ASSEMBLY AND MORPHOLOGICAL OPTIMIZATION OF CRYSTALLINE PRODUCTS, AND PREPARATION OF SAID COMPOUND
Provided is an omeprazole sodium compound prepared by using particle processing for the molecular assembly and morphological optimization of crystalline products. The compound is an omeprazole sodium anhydrous compound, and has a high degree of purity, low hygroscopicity, and excellent fluidity and stability. Also provided is an omeprazole sodium pharmaceutical composition comprising the following components in parts by weight: 20 to 60 parts omeprazole sodium (based on the measurement of omeprazole), 1 to 2 parts metal ion complexing agent and a pH adjusting agent. The omeprazole sodium pharmaceutical composition is simple to prepare, requires no excipient, and has better stability than products of the past.
C07D 401/12 - Composés hétérocycliques contenant plusieurs hétérocycles comportant des atomes d'azote comme uniques hétéro-atomes du cycle, au moins un cycle étant un cycle à six chaînons avec un unique atome d'azote contenant deux hétérocycles liés par une chaîne contenant des hétéro-atomes comme chaînons
A61P 1/04 - Médicaments pour le traitement des troubles du tractus alimentaire ou de l'appareil digestif des ulcères, des gastrites ou des œsophagites par reflux, p. ex. antiacides, antisécrétoires, protecteurs de la muqueuse
A61K 9/19 - Préparations médicinales caractérisées par un aspect particulier à l'état particulaire, p. ex. poudres lyophilisées
A61K 31/4439 - Pyridines non condenséesLeurs dérivés hydrogénés contenant d'autres systèmes hétérocycliques contenant un cycle à cinq chaînons avec l'azote comme hétéro-atome du cycle, p. ex. oméprazole
6.
OMEPRAZOLE SODIUM SEMIHYDRATE AND PREPARATION AND PREPARATION METHOD THEREOF
Disclosed are an omeprazole sodium semihydrate and a preparation method therefor. One mole of omeprazole sodium semihydrate contains 0.5 mole of water, and the X-ray diffraction spectrum thereof has characteristic peaks at diffraction angles 2θ of 6.26±0.1, 11.10±0.1, 12.20±0.1, 15.58±0.1, 16.02±0.1, 17.12±0.1, 19.08±0.1, 21.00±0.1, 22.68±0.1, 23.48±0.1, 24.08±0.1, 26.52±0.1 and 28.08±0.1 degrees. The omeprazole sodium semihydrate is obtained by adding a raw material omeprazole sodium hydrate into an organic solvent, stirring same for 2-9 hours at a constant temperature of 25°C-60°C, and then filtering and drying same. The omeprazole sodium semihydrate of the present invention is high in purity, good in stability, will not easily agglomerate, and has good flowability, and has broader application prospects.
C07D 401/12 - Composés hétérocycliques contenant plusieurs hétérocycles comportant des atomes d'azote comme uniques hétéro-atomes du cycle, au moins un cycle étant un cycle à six chaînons avec un unique atome d'azote contenant deux hétérocycles liés par une chaîne contenant des hétéro-atomes comme chaînons
7.
NEW CRYSTAL FORM OF PANTOPRAZOLE SODIUM COMPOUND AND PREPARATION METHOD THEREFOR
Disclosed are a new crystal form of a pantoprazole sodium compound and a preparation method therefor. The new crystal form is referred to as an M crystal form. The diffraction angle of 2 θ° of X-ray powder diffraction pattern and the characteristic peak of the DSC are used for definition. A pantoprazole sodium solid is added into an alcohol solvent for preparing a suspension liquid of 0.05-0.2 g/mL; an antioxidant is added into the suspension liquid, and the solid is completely dissolved at 15-35°C; a solvating-out agent is added dropwise into the solution under the effect of ultrasound, with the amount of the solvating-out agent being 3-10 times the volume of the alcohol solvent; then the solution is cooled to 0-5°C; stirring is continued for 1-3 h; the formed suspension liquid is filtered by suction; and a pantoprazole sodium crystal product is dried to a constant weight to obtain the new crystal form. The thermal stability test of the product shows that the crystal form product has higher thermal stability. Moreover, the crystal form product has a higher bulk density and better mobility, and facilitates the following preparation process, product storage, transportation and the like.
C07D 401/12 - Composés hétérocycliques contenant plusieurs hétérocycles comportant des atomes d'azote comme uniques hétéro-atomes du cycle, au moins un cycle étant un cycle à six chaînons avec un unique atome d'azote contenant deux hétérocycles liés par une chaîne contenant des hétéro-atomes comme chaînons
A61K 9/28 - DragéesPilules ou comprimés avec revêtements
A61K 9/14 - Préparations médicinales caractérisées par un aspect particulier à l'état particulaire, p. ex. poudres
A61K 31/4439 - Pyridines non condenséesLeurs dérivés hydrogénés contenant d'autres systèmes hétérocycliques contenant un cycle à cinq chaînons avec l'azote comme hétéro-atome du cycle, p. ex. oméprazole
A61P 1/04 - Médicaments pour le traitement des troubles du tractus alimentaire ou de l'appareil digestif des ulcères, des gastrites ou des œsophagites par reflux, p. ex. antiacides, antisécrétoires, protecteurs de la muqueuse
8.
NEW CRYSTAL FORM OF CEFATHIAMIDINE COMPOUND AND PREPARATION METHOD THEREFOR
A new crystal form of a Cefathiamidine compound and a preparation method therefor. The method comprises: dissolving a Cefathiamidine compound with the purity greater than or equal to 98% in a solvent selected from methanol and the like to form a solution with the concentration of 0.05 g/mL to 0.2 g/mL, and dropwise adding in the solution a solvating-out agent selected from n-propyl alcohol and the like; cooling the solution to 0°C to 10°C at a cooling speed of 0.2°C/min to 1°C/min; and continuing to stir for 1 to 3 h, separating the obtained solid-liquid suspension, and drying to obtain the new crystal form product.
C07D 501/28 - Radicaux méthylène substitués par des atomes d'oxygèneLeurs lactones avec le groupe carboxyle-2 avec le radical amino-7 acylé par un acide carboxylique aliphatique, lequel est substitué par des hétéro-atomes
9.
NEW CRYSTALLINE FORM OF CEFAMANDOLE SODIUM COMPOUND, FORMULATION AND PREPARATION METHOD THEREOF
A new crystal form of cefamandole sodium compound and preparation method thereof, the method comprising: adding cefamandole sodium solid to an organic solvent to prepare a 0.04-0.3 g/ml suspension, stirring and suspending for a period of time at 40-50˚C, and then cooling at a certain cooling rate to 5-15˚C and stirring for a period of time, and conducting suction filtration on the obtained suspension to acquire a filter cake, and drying wet crystal product of cefamandole sodium to a constant weight. The appearance of the crystal form is in coarse rod.
A high purity alanyl glutamine compound and preparation method thereof. The high purity product is obtained through gradient recrystallization by using hydrazine compound as an ammoniation reagent with a water/ethanol ratio of 1:1-3.
C07C 237/12 - Amides d'acides carboxyliques, le squelette carboné de la partie acide étant substitué de plus par des groupes amino ayant les atomes de carbone des groupes carboxamide liés à des atomes de carbone acycliques du squelette carboné le squelette carboné étant acyclique et saturé ayant l'atome d'azote d'au moins un des groupes carboxamide lié à un atome de carbone acyclique d'un radical hydrocarboné substitué par des groupes carboxyle
C07C 231/14 - Préparation d'amides d'acides carboxyliques par formation de groupes carboxamide combinée avec des réactions n'impliquant pas les groupes carboxamide
11.
LANSOPRAZOLE COMPOUND AND NOVEL PREPARATION METHOD THEREOF
The present invention provides a refining method of a lansoprazole compound. The method comprises: separating and purifying a rough lansoprazole product by using a macroporous adsorption resin column, performing eluting with an eluting agent and collecting an eluent; carrying out negative-pressure crystallization on the eluent, comprising the following steps of: 1) adding at least half or more eluent containing lansoprazole to a crystallization container, and carrying out concentration under negative pressure and rising temperature; 2) reducing the temperature and adding lansoprazole crystal seeds; 3) when fine crystalline grains appear, causing materials in the crystallization container to be in a boiled concentration state, adding the rest of the eluent to the crystallization container, and holding the temperature for continuous crystallization; and 4) separating, washing and drying the separated crystals to finally obtain refined lansoprazole.
C07D 401/12 - Composés hétérocycliques contenant plusieurs hétérocycles comportant des atomes d'azote comme uniques hétéro-atomes du cycle, au moins un cycle étant un cycle à six chaînons avec un unique atome d'azote contenant deux hétérocycles liés par une chaîne contenant des hétéro-atomes comme chaînons
12.
NOVEL METHOD FOR PREPARING CEFMENOXIME HYDROCHLORIDE COMPOUND
A method for purifying cefmenoxime hydrochloride, comprising specifically the following steps: 1) adding a cefmenoxime hydrochloride-insoluble solvent to a cefmenoxime hydrochloride raw material, removing impurities by filtering; 2) using ammonia for processing, further reducing impurities; 3) using hydrochloric acid to adjust the pH value, acquiring a refined cefmenoxime hydrochloride by low-temperature crystallization; and 4) optionally, returning to step 3) a crystallization mother liquor having crystals precipitated therefrom. The method of the present invention allows for improved purity of cefmenoxime hydrochloride, reduced impurity content, improved preparation product quality, and reduced toxic side effects.
A method for purifying ceftizoxime sodium, comprising (1) dissolving crude ceftizoxime sodium in water, extracting with cyclohexane or ethyl acetate, and acquiring an aqueous phase having ceftizoxime sodium; (2) introducing ammonia or ammonium hydroxide, stirring, filtering, and optionally heating to remove residual ammonia; (3) adding an alcohol solvent, recrystallizing, centrifuging, washing, drying, and acquiring refined ceftizoxime sodium; and (4) optionally, returning a crystallization mother liquor to step (3). The method greatly improves the purity of ceftizoxime sodium and reduces toxic side effects.
C07D 501/20 - Acides acylamino-7 céphalosporaniques ou acylamino-7 céphalosporaniques substitués dans lesquels les radicaux acyle sont dérivés d'acides carboxyliques
A method for purifying cefotiam hydrochloride is provided, which comprises the following steps: step 1) dissolving raw material cefotiam hydrochloride in water, treating the solution with an acidic salt, then decreasing the temperature and filtering the precipitate generated to obtain an aqueous filtrate; step 2) extracting above-said aqueous solution by adding a solvent or solvents immiscible with water into it and then removing off the organic phase containing impurities to obtain the aqueous solution comprising cefotiam hydrochloride; step 3) adding a poor solvent or poor solvents for cefotiam hydrochloride to said aqueous solution, controlling the temperature to recrystallize, centrifuging, washing and drying the educed crystals to get purified cefotiam hydrochloride.
Disclosed herein is a purification method of cefmetazole sodium including processing steps as follows: step 1), dissolve the raw material cefmetazole sodium into water, and extract it by adding water insoluble organic solvent, then discard the organic phase containing impurity and obtain the aqueous phase containing cefmetazole sodium; step 2), treat the said aqueous phase by adding alkali metal or alkaline earth metal alkoxide, then filter the solvent and obtain the filtrate; step 3), recrystallize the solvent by adding ethanol or acetone, then rinse through centrifugation and dry the crystal separated from the solvent to obtain the refined cefmetazole sodium. By the method applied above, the purity of raw material cefmetazole sodium can be substantially enhanced.
A purification method of aztreonam comprises: step 1), in the presence of proper solvents or solvent mixture, processing aztreonam with alkaline alkoxy or alkaline earth alkoxy under heating, then adjusting pH with proper acid, cooling, precipitating aztreonam, obtaining preliminarily purified aztreonam; step 2), adsorping aztreonam with strong basic ion-exchange resin, then eluting, collecting eluent, vacuum concentrating, obtaining secondarily purified aztreonam; step 3), adjusting pH with proper acid, performing crystallization, centrifugating and washing the precipitated crystal, drying, obtaining thirdly purified aztreonam. The purity of obtained aztreonam is not less than 99.2%, most part exhibit a purity not less than 99.5%. The product has very low heavy metal content and has very few calcination residue.
C07D 417/12 - Composés hétérocycliques contenant plusieurs hétérocycles, au moins un cycle comportant des atomes de soufre et d'azote comme uniques hétéro-atomes du cycle, non prévus par le groupe contenant deux hétérocycles liés par une chaîne contenant des hétéro-atomes comme chaînons
Provide a process of refining cefamandole sodium comprising steps as follows: step 1), adsorbing cefamandole sodium by strong acid ion exchange resin, and collecting the eluant after eluting, then decompressing and concentrating to obtain cefamandole acid, step 2), using sodium hydroxide solution or alkaline sodium solution to neutralise and adjust pH, filtering while the solution is hot to remove insoluble material, then obtain cefamandole sodium solution; step 3), adding ethanol into the solution with a water/ethanol volume ratio of 4:6, and controlling the temperature to recrystallization, acquiring purified cefamandole sodium. The refined cefamandole sodium has a purity higher than 99.5%, most of which has a purity higher than 99.6%, and the refined cefamandole sodium has very low heavy metal content.
A61K 31/546 - Composés contenant des systèmes cycliques thia-5 aza-1 bicyclo [4.2.0] octane, c.-à-d. composés contenant un système cyclique de formule , p. ex. céphalosporines, céfaclor, céphalexine contenant d'autres hétérocycles, p. ex. céphalotine
brevets