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A kind of preparation method of cefamandole sodium powder injection preparation

A technology of mendolate sodium powder and preparation, which is applied in the field of medicine, can solve the problems of high content of impurities and long reaction time, and achieve the effects of low content of impurities, short reaction time and low reaction residue

Active Publication Date: 2019-09-24
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is exactly to provide a kind of preparation method of cefamandole sodium powder injection preparation, to solve the problem that existing method reaction time is long and cefamandole, impurity etc. content are high in the product

Method used

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  • A kind of preparation method of cefamandole sodium powder injection preparation

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Experimental program
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Effect test

Embodiment 1

[0026] Into a 500mL four-necked flask, add 75mL of dichloromethane, 25g of 7-TMCA, and 28.8g of BSA, heat up to 35°C, react for 30min, dissolve and clear, and cool down after the reaction. The temperature was controlled to -5~0°C, 15 mL of formyl mandelic acid chloride was added dropwise, and the reaction was performed for 5 minutes after the addition, and the residual 7-TMCA was detected to be less than 2.0%, and the reaction was completed. Add 50 mL of purified water to another four-necked flask, control the temperature below 15°C, add the reaction solution to the four-necked flask, and simultaneously add 15wt% sodium hydroxide solution, control pH=4.8±0.1, and stir rapidly for 5min , stand for phase separation, and recover the organic phase. Add 150 mL of ethyl acetate to the aqueous phase, adjust pH=1.25 with 6 mol / L hydrochloric acid solution, stir rapidly for 10 min, stand for phase separation, and discard the aqueous phase.

[0027] 2.5g of activated carbon and 2.5g of...

Embodiment 2

[0030] Add 150 mL of dichloromethane, 25 g of 7-TMCA, 20.6 g of BSA, and 5.5 g of trimethylchlorosilane into a 500 mL four-neck flask, heat up to 42° C., react for 50 min, dissolve and clear, and cool down after the reaction is completed. The temperature was controlled to -10~-5°C, 15 mL of formyl mandelic acid chloride was added dropwise, and the reaction was carried out for 20 min after the addition, and the residual 7-TMCA was detected to be less than 2.0%, and the reaction was completed. Add 50 mL of purified water to another four-necked flask, control the temperature below 15°C, add the reaction solution to the four-necked flask, and simultaneously add 10wt% sodium bicarbonate solution, control pH=5.5±0.1, and stir rapidly for 5min , stand for phase separation, and recover the organic phase. Add 150 mL of ethyl acetate to the aqueous phase, adjust pH=0.52 with 6 mol / L hydrochloric acid solution, stir rapidly for 10 min, stand for phase separation, and discard the aqueous ...

Embodiment 3

[0034] Into a 500mL four-neck flask, add 125mL of dichloromethane, 25g of 7-TMCA, add 30.5g of BSA, heat up to 30°C, react for 60min, dissolve and clear, and cool down after the reaction. The temperature was controlled to -10~-5°C, and 15 mL of formyl mandelic acid chloride was added dropwise. After the addition, the reaction was performed for 10 min, and the residual 7-TMCA was detected to be less than 2.0%, and the reaction was completed. Add 50 mL of purified water to another four-necked flask, control the temperature below 15°C, add the reaction solution to the four-necked flask, and simultaneously add 10wt% sodium carbonate solution, control pH=6.5±0.1, stir rapidly for 5min, The phases were separated by standing, and the organic phase was recovered. Add 150 mL of ethyl acetate to the aqueous phase, adjust pH=1.35 with 6 mol / L hydrochloric acid solution, stir rapidly for 10 min, stand for phase separation, and discard the aqueous phase.

[0035] 2.5 g of activated carbon...

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Abstract

The invention provides a method for preparing a cefamandole nafate powder injection preparation. The method comprises the following steps: (a) performing a silanization reaction on 7-ACT and a silanization agent in a dichloromethane solvent under temperature control, and reducing the temperature after the reaction is completed so as to obtain a reaction liquid 1, wherein the solid-liquid ratio of7-ACT to dichloromethane is 1g:(3-6)ml; (b) dropwise adding (R)-(-)-O-formylmandeloyl chloride into the reaction liquid 1, controlling the temperature, performing an acylation reaction so as to obtaina reaction liquid 2; (c) performing treatment of extraction, decoloring and dehydration on the reaction liquid 2; (d) performing temperature control crystallization; and (e) washing a solid with acetone, drying, performing sterile sub-packaging, thereby obtaining the cefamandole nafate powder injection preparation. Due to adoption of a high-concentration dichloromethane reaction system, the method is rapid in silanization and acylation process, short in reaction time, low in reaction residue, high in product yield and small in impurity. After the reactions, organic solvents such as dichloromethane can be easily recycled and repeatedly used, so that the method is relatively environment-friendly, low in cost and applicable to large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of a cefamandole sodium powder injection preparation. Background technique [0002] Cefamandole sodium belongs to the second generation cephalosporin antibiotics, the chemical name is 7-D-(2-formyloxyphenylacetamide)-3-[(1-methyl-1H-tetrazol-5-yl) Mercaptomethyl]-3-cephem-4-carboxylate sodium salt, is the prodrug of cefamandol. After intravenous or intramuscular injection, it is rapidly hydrolyzed into the active ingredient cefamandol in the body, with fewer side effects and better safety. It is widely recognized by clinicians for its advantages of high efficacy and relatively precise curative effect, and is suitable for pulmonary infection, urinary tract infection, biliary tract infection, skin and soft tissue infection, bone and joint infection, sepsis, abdominal infection, etc. caused by sensitive bacteria. [0003] Cefmandole sodium was succ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/06C07D501/12
Inventor 胡利敏石春利李庆伟贾全刘树斌任峰田洪年郭振军林建新张红蕾李惠芬贾丽辉李萌
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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