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Cefpiramide sodium hydrate and preparation method and application thereof

A technology of cefpiramide sodium and hydrate, applied in the field of medicine, can solve the problems of reporting the preparation method and use of cefpiramide sodium crystal hydrate, and achieve the effects of improving operability, good sliding property, and being convenient for storage and transportation

Inactive Publication Date: 2010-09-22
胡梨芳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, published literature only reports cefpiramide sodium (Cefpiramide sodium) (C 25 h 23 N 8 NaO 7 S 2 , Molecular Weight: 634.62, CAS No.: 74849-93-7), up to now, there is no published literature at home and abroad to report cefpiramide sodium crystalline hydrate of the present invention and its preparation method and use

Method used

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  • Cefpiramide sodium hydrate and preparation method and application thereof
  • Cefpiramide sodium hydrate and preparation method and application thereof
  • Cefpiramide sodium hydrate and preparation method and application thereof

Examples

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Embodiment 1

[0037] Example 1 Preparation of Cefpiramide Sodium Monohydrate Add 10 g of cefpiramide, 20 ml of water, and 30 ml of methanol in a reaction flask, stir, add 2.4 ml of triethylamine dropwise with stirring at 5° C., stir for 30 minutes, add 0.1 ml of activated carbon g, stirred for 30 minutes, filtered with suction, washed with water, filtered with suction, added dropwise an ethanol solution of 25% sodium isooctanoate (2.8g) in the filtrate at 5°C, stirred, slowly added 250ml of acetone and 250ml of ethanol dropwise, below -6°C Put it aside to allow the solid to be fully separated, filter with suction, wash with a small amount of chloroform for 3 times, and filter with suction, dissolve the obtained solid with a small amount of water, add 300ml of acetone and 300ml of isopropanol for recrystallization, and place it below -6°C to make the solid fully Precipitate, filter with suction, wash with a small amount of chloroform for 3 times, filter with suction, and dry the obtained soli...

Embodiment 2

[0038]Example 2 Preparation of Cefpiramide Sodium Monohydrate Add 20 g of cefpiramide sodium and 80 ml of water into the reaction flask, stir to form a suspension, add saturated aqueous sodium carbonate solution dropwise at 5°C to make the pH to about 6.8, and stir For 30 minutes, add 0.5g of activated carbon, stir for 30 minutes, filter with suction, wash with water, filter with suction, slowly add 250ml of acetone and 300ml of acetonitrile dropwise, place below -4°C to fully separate out the solid, filter with suction, wash with acetone for 3 times, and filter with suction , the resulting solid was just dissolved with a small amount of water, recrystallized with 300ml of acetone, 300ml of acetonitrile, and 10ml of chloroform, and placed overnight below -10°C to allow the crystals to be fully separated, filtered with suction, washed with a small amount of acetone for 3 times, filtered with suction, and kept at 52°C Vacuum-dried for about 6 hours to obtain 13.4 g of off-white c...

Embodiment 3

[0039] Example 3 Preparation of Cefpiramide Sodium 1.5 Hydrate Add 20 g of cefpiramide and 80 ml of water into the reaction flask, stir to form a suspension, add dropwise a saturated aqueous solution of sodium bicarbonate under stirring at 5°C to bring the pH to about 6.8, and stir 30 minutes, add 0.3g of activated carbon, stir for 30 minutes, filter with suction, wash with water, filter with suction, slowly add 350ml of acetone and 250ml of ethanol, place below -5°C, let the solid fully separate out, filter with suction, wash with ethanol 3 times, and filter with suction , the obtained solid was just dissolved with a small amount of water, added 300ml of ethanol, 300ml of acetonitrile, and 80ml of isopropyl ether as a crystallization solvent for recrystallization, and placed overnight below -10°C to fully separate out the crystals, suction filtered, and vacuum-dried at 45°C at 0.06MPa About 5 hours, 10.6g of off-white crystals were obtained, melting point: discoloration at 170...

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Abstract

The invention relates to a cefpiramide sodium hydrate and a preparation method and application thereof. The cefpiramide sodium hydrate has high storage stability, and is applicable to the preparation of medicines for treating or preventing diseases of the human being or animals caused by gram-positive or gram-negative sensitive bacteria, such as respiratory system diseases, hepatobiliary system diseases, five-sense organ diseases, urinary tract infection, celiac infection, pelvic infection, ichorrhemia, skin tissue infection, bone and joint infections, endocarditis and cephalomeningitis.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to provide antibacterial drug-cefepiramide sodium hydrate and its preparation method and application. Background technique [0002] Cefpiramide sodium is a cephalosporin jointly developed by Japan's Sumitomo Pharmaceutical Company and Yamanouchi Pharmaceutical Company. According to the principle of cephalosporin discovery age and antibacterial properties, the drug is between the third generation and the fourth generation. During the period, some people called it "three and a half generations" of cephalosporins. Cefpiramide sodium was first listed in Japan in 1985, and then in other countries such as the United States. Its structural feature is that there is a methyl tetrazolium thio group at the C3 position, and a hydroxyphenyl group and a hydroxymethylpyridyl group at the C7 position, thus greatly improving the antibacterial activity and pharmacokinetic characteristics of the ori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/04A61K31/546A61K31/431A61K31/424A61K31/43A61P31/04
CPCC07D501/36A61K31/546A61P31/04
Inventor 刘力
Owner 胡梨芳
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