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Special ultrafine cefmetazole sodium powder preparation and preparation method thereof

A technology of cefmetazole sodium and ultrafine powder, which is applied in the field of medicine, can solve the problems of low clarity, small specific surface area, and large toxic and side effects of cefmetazole sodium, achieve good clarity, large specific surface area, and improve utilization rate effect

Inactive Publication Date: 2014-11-26
杭州长典老一元健康管理有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing cefmetazole sodium has the disadvantages of low clarity, poor stability, low purity, many impurities, large particles, small specific surface area, poor solubility, large toxic and side effects, and easy allergies

Method used

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  • Special ultrafine cefmetazole sodium powder preparation and preparation method thereof
  • Special ultrafine cefmetazole sodium powder preparation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 30 grams of cefmetazole benzyl ester to 150 grams of dichloromethane, cool to -30°C to avoid side reactions, then add 330 grams of anisole and 60 grams of ferric chloride, Carry out the reaction, when cefmetazole benzyl axetil remains ≤ 1.0%, the reaction is considered to be over, the reaction solution is stirred and then added to a mixed solution consisting of 8% hydrochloric acid solution 250ml (259g) and acetone 306ml (240g), After stirring for 30 minutes, the layers were left to stand, and the organic phase was collected. The organic phase was poured into 250ml of 8% sodium chloride solution, stirred and allowed to stand for layering, and the organic phase was collected.

[0024] Add 3% sodium bicarbonate solution to the organic phase, adjust the pH to 7, stir for 20 minutes, let stand to separate layers, collect the water phase, adjust the pH of the water phase to 5.5 with acetic acid, then add 3 grams of activated carbon, and stir for 30 minutes to decolorize ...

Embodiment 2

[0030] Add 30 grams of cefmetazole benzyl ester to 225 grams of dichloromethane, cool to -25°C to avoid side reactions, then add 390 grams of anisole and 75 grams of ferric chloride, Carry out the reaction, when cefmetazole benzyl axetil remains ≤ 1.0%, the reaction is considered to be over, the reaction solution is stirred and then added to a mixed solution consisting of 220ml (230g) of 10% hydrochloric acid solution and 344ml (270g) of acetone, After stirring for 30 minutes, the layers were left to stand, and the organic phase was collected. The organic phase was poured into 250ml of 10% sodium chloride solution, stirred and allowed to stand for layering, and the organic phase was collected.

[0031] Add 5% sodium bicarbonate solution to the organic phase, adjust the pH to 7.5, stir for 20 minutes, let it stand for stratification, collect the water phase, adjust the pH of the water phase to 6 with acetic acid, then add 6 grams of activated carbon, and stir for 30 minutes to dec...

Embodiment 3

[0037] Add 30 grams of cefmetazole benzyl ester to 300 grams of dichloromethane, cool to -20°C to avoid side reactions, then add 450 grams of anisole and 90 grams of ferric chloride, Carry out the reaction, when cefmetazole benzyl axetil remains ≤ 1.0%, the reaction is considered to be over, the reaction solution is stirred and then added to a mixed solution consisting of 200ml (211g) of 12% hydrochloric acid solution and 382ml (300g) of acetone, After stirring for 30 minutes, the layers were left to stand, and the organic phase was collected. The organic phase was poured into 250 ml of a 12% sodium chloride solution, stirred and allowed to stand for layering, and the organic phase was collected.

[0038] Add 8% sodium bicarbonate solution to the organic phase, adjust the pH to 8, stir for 20 minutes, let it stand for stratification, collect the water phase, adjust the pH of the water phase to 6.5 with acetic acid, then add 9 grams of activated carbon, and stir for 30 minutes t...

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Abstract

The invention discloses a special ultrafine cefmetazole sodium powder preparation and a preparation method thereof. The preparation method comprises the following steps: carrying out a reaction on a raw material cefmetazole benzyl ester in a dichloromethane, anisole and iron trichloride system, carrying out acidolysis by using a hydrochloric acid and acetone mixed solution, purifying the above collected organic phase by using a sodium chloride solution, carrying out phase inversion by using a sodium bicarbonate solution, decoloring the above collected water phase by active carbon and alumina, carrying out phase inversion by ethyl acetate and hydrochloric acid, crystallizing by adding crystal seeds in order to prepare cefmetazole acid, reacting cefmetazole acid with sodium bicarbonate to prepare cefmetazole sodium, purifying, and carrying out air jet ultrafine crushing to prepare the special ultrafine cefmetazole sodium powder preparation. The special ultrafine cefmetazole sodium powder preparation has the advantages of good clarity, high stability, high purity, few impurities, small particle size, large specific surface area, good solubility, small toxic side effects, difficult allergy and the like.

Description

technical field [0001] The invention relates to a special ultrafine powder preparation of cefmetazole sodium and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Cefmetazole sodium, its English name is Cefmetazole Sudium, its chemical name is (6R,7S)-7-[2-[(cyanomethyl)thio]acetamido]-7-methoxy-3-[[ (1-methyl-1H-tetrazol-5-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2- Sodium carboxylate. Molecular formula is C 15 h 16 N 7 NaO 5 S 3 , the molecular weight is 493.52. [0003] Cefmetazole sodium is a second-generation cephalosporin, a semi-synthetic cephalosporin antibiotic created by Japan Sankyo Co., Ltd., which has good stability to the broad-spectrum β-lactamase produced by negative bacilli. Escherichia coli, Klebsiella pneumoniae, Proteus mirabilis, Shigella, Salmonella and other negative bacilli have good sensitivity to this product. Staphylococcus aureus, group A hemolytic streptococcus, and...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/04A61K31/546A61P31/04
CPCC07D501/57C07D501/04
Inventor 傅苗青李凤生厉达中
Owner 杭州长典老一元健康管理有限公司
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