Cefoperazone sodium compound entity, composition and application

A kind of technology of cefoperazone sodium and compound, which is applied to the new compound entity and composition of cefoperazone sodium and the field of preparation thereof, and achieves the effects of improving operability, good sliding property, convenient storage and transportation

Inactive Publication Date: 2015-02-04
LIANHE KANGXING BEIJING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Up to the present, there is no published bibliography at home and abroad to report cefoperazone sodium crystalline hydrate of the present invention and its preparation method and application etc.

Method used

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  • Cefoperazone sodium compound entity, composition and application
  • Cefoperazone sodium compound entity, composition and application
  • Cefoperazone sodium compound entity, composition and application

Examples

Experimental program
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Embodiment 1

[0063] The preparation of embodiment 1 cefoperazone sodium 1.5 hydrate

[0064] Add 10g of cefoperazone acid, 85m of ethanol, and 3ml of water into a 500ml flask, stir to dissolve, add 0.1g of activated carbon, stir for 30 minutes, filter with suction, add a mixed solution of sodium carbonate and ethanol dropwise to the filtrate at 5°C, and stir , adjust the pH to about 7.0 with glacial acetic acid, slowly add 50ml of acetone and 250ml of ethanol dropwise, and place it below -4°C to allow the solid to fully separate out, filter with suction, wash with a small amount of cold ethanol and chloroform for 3 times, filter with suction, and dissolve the obtained solid with an appropriate amount of water , Add 240ml of ethanol and 30ml of acetone as the crystallization solvent for recrystallization, place it below 5°C for about 2 hours, then place it at 0~-4°C for about 3 hours, and place it at about -10°C overnight, so that the crystals can be fully analyzed. Filter, wash with a smal...

Embodiment 2

[0065] The preparation of embodiment 2 cefoperazone sodium 1.5 hydrate

[0066] Add 20g of cefoperazone acid and 50ml of water into a 250ml flask, stir to form a suspension, add dropwise 20ml of an aqueous solution of 2.9g of anhydrous sodium carbonate at 15°C, stir to dissolve, add 0.2g of activated carbon, stir for 30 minutes, and pump Filtrate, wash with water, and suction filter, adjust the pH of the filtrate to about 7.2 with glacial acetic acid, then slowly add 100ml of acetone, 250ml of ethanol, and 5ml of isopropyl ether dropwise, and place it below 0°C to allow the solids to fully separate out, then filter with suction, and add a small amount of ethanol, acetone and Wash 3 times with chloroform, filter with suction, dissolve the obtained solid with an appropriate amount of water, use 80ml of acetone, 230ml of ethanol, 10ml of isopropanol, and 5ml of isopropyl ether as the crystallization solvent for recrystallization, place it below 5°C for about 3 hours, and then plac...

Embodiment 3

[0067] The preparation of embodiment 3 cefoperazone sodium 2 hydrates

[0068] Add 10g of cefoperazone acid and 30ml of water into a 250ml flask, stir to form a suspension, add a saturated aqueous solution of sodium bicarbonate dropwise at 10°C until the pH is about 7.0, stir to dissolve, add 0.2g of activated carbon, and stir for 30 minutes. Suction filtration, washing with water, suction filtration, slowly dropwise add 10ml of chloroform, 300ml of acetone, 20ml of isopropanol to the filtrate and place it below 10°C to allow the solid to be fully separated out, suction filtration, washing with a small amount of ethanol for 3 times, suction filtration, and the obtained solid with an appropriate amount of Dissolve in water, 300ml of acetone, 10ml of chloroform, 20ml of isopropanol as crystallization solvent for recrystallization, place at about 8°C for about 2 hours, then place at -4°C for about 3 hours, and place at -15°C for about 10 hours , the crystals were fully separated,...

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Abstract

The invention provides a cefoperazone sodium compound entity and a composition thereof. The cefoperazone sodium compound entity is low in hygroscopicity and good in storage stability, is suitable in an application of preparing drugs for treating or preventing respiratory system infection, infection in the five sense organs, urinary system infection, pelvic cavity infection, septicemia, skin soft tissue infection, infection in bones and joints, gonorrhea and meningitis of human or animal due to bacteria being sensitive to gram-positive bacteria or gram-negative bacteria.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to provide a new compound entity and composition of the antibacterial drug cefoperazone sodium as well as its preparation method and application. Background technique [0002] Polymorphic forms of chemical drugs play an important role in drug research. In the field of pharmacology, the research work on drug crystal forms and drug hydrates or drug solvates has been listed in the research scope of the National Twelfth Five-Year Major New Drug Innovation Science and Technology Major Project. Solvents of compounds, including hydrates, have been prepared and used in medicines for a long time. For example, the anti-tumor drug cyclophosphamide recorded in the 36th edition of the US Pharmacopoeia, the 6.1th edition of the European Pharmacopoeia, and the 2010 edition of the Chinese Pharmacopoeia can only be used in solids at room temperature. Existing in the form of monohydrate, the compou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36A61K31/546A61P31/04A61K31/424A61K31/43A61K31/431
CPCC07D501/36C07B2200/13C07D501/04C07D501/12
Inventor 刘力
Owner LIANHE KANGXING BEIJING PHARMA
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