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A kind of technique for preparing cefathiamidine

A cefathiamidine and process technology, applied in the field of chemical drug synthesis, can solve the problem of high residual amount of impurities, achieve the effects of high reaction yield, avoid side reactions and reduce the content of impurities

Active Publication Date: 2018-08-14
山西振东泰盛制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to solve the technical problem of high residual impurities in the existing process for preparing cefathiamidine, the present invention provides a method for preparing cefathiamidine that effectively reduces residues of bromoacetyl-7ACA and high molecular impurities

Method used

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  • A kind of technique for preparing cefathiamidine
  • A kind of technique for preparing cefathiamidine
  • A kind of technique for preparing cefathiamidine

Examples

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Embodiment 2

[0039]In a 10L reactor, add DCM 5320 g (4L), TEA (200mL), bromoacetyl-7ACA 500g in sequence, stir to dissolve, add co-solvent pure water 50mL, then add N,N-diisopropylthiourea 225 g. After stirring and dissolving, heat the reaction liquid to reflux. After reacting for 2-3 hours, stop the reaction and lower the internal temperature to 0°C-15°C. Add 2L of acetone dropwise, stir and crystallize. After the dropwise addition, keep stirring at 8-12°C and filter with suction. After the filter cake is drained, add 1L of acetone to rinse the filter cake. After draining, add the filter cake to 10L Then add 600mL of pure water and stir to dissolve, then add 1080 g (1.2L) of ethyl acetate, stir for 10 minutes, extract impurities, after standing for layers, filter the water layer into the crystallization reactor, and use dilute Adjust the pH of the solution to 5.0 with hydrochloric acid, cool the obtained clear mixed solution to 0-5°C, add 5.6L of acetone dropwise, after the dropwise addit...

Embodiment 3

[0041] Add 400 mL of DCM, 18 mL of TEA, and 50 g of bromoacetyl-7ACA to a 1L reaction flask in sequence, stir to dissolve, add 10 mL of co-solvent pure water, then add 22.5 g of N,N-diisopropylthiourea, and stir to dissolve Afterwards, heat the reaction liquid to reflux, react for 2-3 hours, stop the reaction, add 10 mL of pure water as a co-solvent, and lower the internal temperature to 10°C to 15°C. Add 200mL of acetone dropwise, stir and crystallize. After the dropwise addition, keep stirring at 8-12°C and filter with suction. After the filter cake is drained, add 100mL of acetone to rinse the filter cake. into the reaction flask, then add 60 mL of pure water and stir to dissolve, then add 108 g (120 mL) of ethyl acetate, stir for 10 minutes, extract impurities, stand to separate the layers, filter the water layer into the crystallization reaction flask, and use dilute Adjust the pH of the solution to 4.5 with hydrochloric acid, cool the obtained clear mixed solution to 0-5...

Embodiment 4

[0043] Add 400 mL of DCM, 20 mL of TEA, and 50 g of bromoacetyl-7ACA to a 1L reaction flask in sequence, stir to dissolve, then add 22.5 g of N,N-diisopropylthiourea, stir to dissolve, then heat the reaction solution to reflux , After reacting for 2-3 hours, stop the reaction and lower the internal temperature to 10°C to 15°C. Add 200mL of acetone dropwise, stir and crystallize. After the dropwise addition, keep stirring at 8-12°C and filter with suction. After the filter cake is drained, add 100mL of acetone to rinse the filter cake. Then add 60 mL of pure water and stir to dissolve, then add 108 g (120 mL) of ethyl acetate, stir for 10 minutes, extract impurities, stand to separate layers, filter the water layer into the crystallization reaction bottle, and use dilute Adjust the pH of the solution to 5.0 with hydrochloric acid, cool the obtained clear mixture to 0-5°C, add 560mL of acetone dropwise, after the dropwise addition, keep stirring at 0-5°C for 30min, filter with s...

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Abstract

The present invention relates to a process for preparing cefathiamidine, in particular a process for preparing high-purity cefathiamidine. The preparation method comprises the following steps of: adding water or an aqueous inorganic salt solution as an auxiliary solvent in or after a reaction on acetyl bromide-7ACA and N,N'-diisopropylthiourea; after the reaction, cooling the mixture, and dropwise adding a crystallization solvent into the mixture, and performing suction filtration to obtain a crude product of cefathiamidine; and purifying the crude product again,and drying the crude product in vacuum to obtain the high-purity cefathiamidine. According to the preparation method provided by the present invention, residues of impurities in the cefathiamidine can be effectively reduced, the content of acetyl bromide-7ACA and the macromolecular compound impurities can be reduced to 0.1% or less or can be completely eliminated, and other residues of impurities in the cefathiamidine can be reduced to be less than 0.2%.

Description

technical field [0001] The invention belongs to the field of chemical drug synthesis, and relates to a preparation method of high-purity cefathiamidine, in particular to a method for preparing cefathiamidine with high-purity cefathiamidine which reduces the impurity content by using bromoacetyl-7ACA and polymer compounds craft. Background technique [0002] Cefathiamidine is a β-lactam antibiotic independently developed by Shanghai Pharmaceutical Industry Research Institute and Guangzhou Baiyunshan Pharmaceutical Co., Ltd. It has strong antibacterial effect on most Gram-positive bacteria and some Gram-negative bacteria. role, especially for enterococci have a unique effect. It is widely used clinically, mainly for respiratory tract infection and biliary tract infection caused by Staphylococcus aureus, pneumococcus and streptococcus. [0003] The structural formula is as follows: [0004] [0005] At present, the intermediate bromoacetyl-7ACA produced by the reaction of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/28C07D501/04
CPCC07D501/04C07D501/28
Inventor 高治华赵永军张涛梁波熊继业沈达
Owner 山西振东泰盛制药有限公司
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