Ceftizoxime sodium drug injection powder and preparation method thereof, as well as synthetic method of bulk drug ceftizoxime sodium

A technology of cefizoxime sodium and cefizoxime acid is applied in the field of drug synthesis and preparation, and can solve the problems of complex chromatography column method, difficult operation and the like

Active Publication Date: 2009-12-23
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method combines the middle sub-chromatographic column and recrystallization that are usually used for material analysis and separation technology to purify ceftizoxime or its salt, especially sodium salt. Although high-purity ceftizoxime sodium drug is obtained, the layer The column analysis method is complex and difficult to operate

Method used

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  • Ceftizoxime sodium drug injection powder and preparation method thereof, as well as synthetic method of bulk drug ceftizoxime sodium
  • Ceftizoxime sodium drug injection powder and preparation method thereof, as well as synthetic method of bulk drug ceftizoxime sodium
  • Ceftizoxime sodium drug injection powder and preparation method thereof, as well as synthetic method of bulk drug ceftizoxime sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0114] [embodiment 1] preparation of aminothioxime acetyl chloride

[0115] Put 25.2g of dimethylformamide, 55.1g of phosphorus oxychloride, and 600ml of dry ethyl acetate into the flask. Control the temperature in an ice-water bath at 0-5°C, add 68.1 g of 2-(2-imino-4-thiazolyl)-2-methoxyiminoacetic acid (aminothioxime acetic acid) in batches, and continue the reaction at 0-5°C after adding 1 hour. The solvent was evaporated to dryness under reduced pressure in a water bath at 50°C, and the obtained oil was dissolved in 80ml of acetone for later use.

Embodiment 2

[0116] [Example 2] Preparation of Ceftizoxime Acid

[0117] Add 500ml of water and 14.1g of sodium hydroxide to another flask, and stir to dissolve. Put 67.0 g of 7-amino-3-norcephalosporanic acid into the flask, and adjust the pH value to 12-13 with 5% sodium hydroxide. Cool down to -20~-10°C in an ice-salt bath, and slowly add the prepared aminothioxime acetyl chloride solution dropwise into the flask. During the reaction, control the pH value to 12~13, and the dropwise addition is completed in about 1 hour. After the addition, continue to react at -20~-10°C for half an hour, then raise the temperature to 0°C and react for another hour.

[0118] After the reaction, diethyl ether was added to extract twice, each time with 250 ml of diethyl ether, the layers were separated, and the organic layer was discarded. The aqueous layer was adjusted to pH 1.5 with 10% hydrochloric acid, extracted twice with ethyl acetate, each time with 750 ml of ethyl acetate, and the organic layers...

Embodiment 3

[0119] [Example 3] Preparation of Ceftizoxime Sodium Crude Product

[0120] Put 71.0 g of ceftizoxime acid and 130 ml of water into the flask, control the temperature in an ice-water bath at 0-5°C, and adjust the pH value to 7.0-7.5 with 3 mol / L sodium hydroxide. Add 10.0 g of activated carbon, and stir for 30 minutes at 20-30°C. Suction filtration, and slowly add 1500ml of absolute ethanol to the filtrate under stirring, and the addition is completed in about 30 minutes, and a large amount of white precipitates precipitate out. Refrigerated and crystallized at 0-5°C for 2 hours, filtered, rinsed with 100ml of absolute ethanol, drained, and the filter cake was dried under reduced pressure at 30°C to obtain 62.1g of crude ceftizoxime sodium, with a yield of 82.7%.

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Abstract

The invention relates to a ceftizoxime sodium drug injection powder and a preparation method thereof, as well as a synthetic method of bulk drug ceftizoxime sodium. The ceftizoxime sodium drug injection powder consists of 100% ceftizoxime sodium, wherein the ceftizoxime sodium is pretreated, and the pretreatment is aseptic refining and/or grinding. The ceftizoxime sodium drug has the advantages of high purity, almost no impurity, better and more stable quality, better clarity and the like; and the synthetic method of bulk drug ceftizoxime sodium has lower bulk cost, less synthesis technology difficulty, mild reaction condition, stable and reliable yield and quality, and high purity and yield of products.

Description

technical field [0001] The invention belongs to the field of drug synthesis and preparations, and more specifically, the invention relates to a drug powder injection of ceftizoxime sodium, a preparation method thereof, and a method for synthesizing the raw drug ceftizoxime sodium. Background technique [0002] Ceftizoxime sodium (ceftizoxime sodium) was developed by Japan Tengze Pharmaceutical Industry Co., Ltd., and was first listed in Japan in 1982 under the trade name of ceftizox. This product is a third-generation cephalosporin antibiotic with broad-spectrum antibacterial activity and is stable against broad-spectrum lactamase (including penicillinase and cephalosporinase) produced by various Gram-positive and Gram-negative bacteria. This product has a strong antibacterial effect on Escherichia coli, Klebsiella pneumoniae, Proteus mirabilis and other Enterobacteriaceae bacteria. Pseudomonas such as Pseudomonas aeruginosa and Acinetobacter are less sensitive to this produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K9/14A61K31/546A61P31/04C07D501/22
Inventor 李明华孙松刘明霞
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD
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