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Preparation method for cefmetazole sodium

A technology for cefmetazole sodium and cefmetazole acid, which is applied in the field of preparation of cefmetazole sodium, can solve the problems of long production cycle, low product purity and high content of related substances, and achieves excellent product quality, high purity, and improved product quality. quality effect

Active Publication Date: 2015-04-29
福安药业集团重庆博圣制药有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent application CN102127095A discloses a preparation method of cefmetazole sodium. After reacting cefmetazole acid and sodium isooctanoate, the finished product is obtained by crystallization, washing, and drying. This method uses a large amount of organic solvents, and the content of related substances is relatively high
Cefmetazole sodium is obtained by freeze-drying, which avoids a large amount of use of organic solvents, but this method needs to go through the steps of crystallization and drying of cefmetazole acid, the production cycle is relatively long, and bicarbonate is added to the cefmetazole acid solution Sodium, after lyophilization to obtain cefmetazole, the resulting product has a lower purity

Method used

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  • Preparation method for cefmetazole sodium

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Experimental program
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Effect test

Embodiment 1

[0039] In a dry and clean three-necked flask, add 50g of 7-MAC and 600ml of chloroform, stir to dissolve, cool to -15°C, add 14g of pyridine, dropwise add 18g of cyanomethylmercaptoacetyl chloride, after the addition is complete, stir for 1 hour, add purified water: chlorine Sodium chloride: 40ml of a mixed solution of concentrated hydrochloric acid (9:1:2) was used to stop the reaction, and the layers were separated, and the organic phase was taken, dried, and concentrated to obtain 57.7g of cefmetazole diphenylmethyl ester, with a molar yield of 95%, HPLC 99.0% purity.

[0040] Cefmetazole diphenylmethyl ester purity test conditions (the same below): use octadecylsilane bonded silica gel as filler; use phosphate buffer (take 2.72g of potassium dihydrogen phosphate, add water to dissolve and dilute to 1000ml)- Acetonitrile (50:50) is the mobile phase; the detection wavelength is 214nm, and the resolution of the Mz-2 peak and the adjacent impurity peak should meet the requirem...

Embodiment 2

[0045] In a dry and clean three-neck flask, add 50g of 7-MAC, add 600ml of chloroform and stir to dissolve, cool to -15°C, add 10g of dimethylaminopyridine, dropwise add 18g of cyanomethylthioacetyl chloride, after the addition is complete, stir for 1 hour, add Purified water: 45ml of mixed solution of sodium chloride:concentrated hydrochloric acid (9:1:2) to stop the reaction, leave to stand and separate layers, take the organic phase, dry and concentrate to obtain 58.1g of cefmetazole diphenylmethyl ester, molar yield 95.7%, HPLC purity 99.3%.

[0046] Take 800ml of dichloromethane and cool down to 5-10°C, add 45g of aluminum trichloride under stirring, add 115g of anisole dropwise, control the temperature at 15-20°C, and cool down to -20~-25°C after adding; keep stirring and add cephalosporin 50g of methazole diphenylmethyl ester, react for 0.5 hours, add 50ml of a mixture of acetone:water:concentrated hydrochloric acid (weight ratio 8:8.2:1) cooled to below 0°C to terminat...

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Abstract

The invention discloses a preparation method for cefmetazole sodium. The preparation method for the cefmetazole sodium comprises the following operation steps: (1), adding chloroform to 7-MAC as an initial raw material, stirring and dissolving; adding alkali, dropping cyanomethylthioacetyl chloride, and stirring to react to obtain cefmetazole diphenylmethyl ester; (2), enabling the cefmetazole diphenylmethyl ester obtained in the step (1) to react in an alchlor-anisole system to obtain an organic solution of cefmetazole acid; (3), preparing a sodium bicarbonate solution with the concentration of 5-20 wt%, controlling the temperature within a range from 5 DEG C below zero to 10 DEG C, adding the organic solution of cefmetazole acid, which is obtained in the step (2), stirring, leaving a mixture to stand and layer, taking out a water layer, adding activated carbon, stirring to decolorize, controlling the temperature to 0-5 DEG C, adding neutral alumina, stirring to decolorize, filtering to obtain a filtrate, and freeze-drying the filtrate to obtain the cefmetazole sodium. The preparation method for the cefmetazole sodium has the advantages of high yield, excellent product quality and convenience in industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of cefmetazole sodium. Background technique [0002] Cefmetazole sodium, developed by Japan Sankyo Pharmaceutical Co., Ltd., belongs to the second-generation cephalosporin antibiotics (the structural formula is shown below). It was first listed in Japan in 1980. It is a broad-spectrum, high-efficiency, and low-toxicity antibiotic. It has antibacterial effect on Gram-positive and negative bacteria and anaerobic bacteria, and has good antibacterial activity on Staphylococcus, hemolytic streptococcus, Escherichia coli, Klebsiella pneumoniae, indole-negative and positive Proteus, etc. . [0003] [0004] The structural formula of cefmetazole sodium [0005] Chinese patent application CN102127095A discloses a preparation method of cefmetazole sodium. After reacting cefmetazole acid and sodium isooctanoate, the finished product is obtain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/57C07D501/04
CPCC07D501/04C07D501/57
Inventor 谭超唐劲郭子维包丹谭华明张雄
Owner 福安药业集团重庆博圣制药有限公司
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