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Preparation method of ceftiofur hydrochloride

A technology of ceftiofur hydrochloride and cefuroxime, which is applied in a preparation field of ceftiofur hydrochloride, can solve the problems of environmental pollution, high production cost and high cost, and achieve the effects of reducing environmental pollution and production cost

Inactive Publication Date: 2013-03-27
RINGPU TIANJIN BIOLOGICAL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Chinese patent CN101108855A, disclosed on January 23, 2008, discloses a kind of preparation method of ceftiofur acid, precipitates ceftiofur product in organic solvent and water, freezes and dries, has improved product quality, but product must be freeze-dried, production high cost
This method has the advantage of simple operation, but it uses a large amount of organic solvent (25 times), and the amount of water accounts for 1-20% of the total solvent, which is costly and easy to cause environmental pollution

Method used

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  • Preparation method of ceftiofur hydrochloride
  • Preparation method of ceftiofur hydrochloride
  • Preparation method of ceftiofur hydrochloride

Examples

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Effect test

Embodiment 1

[0029] The synthesis of embodiment 1 ceftiofur hydrochloride

[0030] Add 50 g of cefuroxime and 300 mL of dichloromethane into a 1000 mL three-necked reaction flask, cool the mixture to 5°C, add 29.7 g of triethylamine dropwise, and finish adding dropwise in 20 minutes, then add AE-activator in batches after stirring for 20 minutes Add 77 g of water to 77 g of ester, add 15 mL of water, keep stirring at 5°C for 3 hours, extract twice with 300 mL of water, combine the water phases, add 10 g of activated carbon to decolorize for 30 min, filter, add 30 mL of 5 mol / L hydrochloric acid to the filtrate to adjust the pH value to 1.7 , filtered to obtain a solid wet product, which was dissolved in 500 mL of acetone, and 23 mL of 5 mol / L hydrochloric acid was added dropwise under stirring to adjust the pH value to 1.0, and 1750 mL of water was slowly added dropwise, and solids were gradually precipitated, stirred for 30 min, and left to stand After 2 h, it was filtered, and the solid ...

Embodiment 2

[0031] The synthesis of embodiment 2 ceftiofur hydrochloride

[0032] Add 40 g of cefuroxime and 240 mL of dichloromethane into a 1000 mL three-necked reaction flask, cool the mixture to 0°C, add 17.8 g of triethylamine dropwise, finish adding dropwise in 20 minutes, and add AE-activator in batches after stirring for 20 minutes Add 12 mL of water to 41.2 g of ester, keep stirring at 0°C for 3 hours, extract twice with 250 mL of water, combine the water phases, add 8 g of activated carbon to decolorize for 30 min, filter, add 23 mL of 5 mol / L hydrochloric acid to the filtrate to adjust the pH value 1.7, filter to obtain a solid wet product, dissolve it in 640 mL of acetone, add 18 mL of 5 mol / L hydrochloric acid dropwise under stirring to adjust the pH value to 1.0, slowly add 1790 mL of water dropwise, gradually a solid precipitates out, stir for 30 min, Let stand for 2 h, filter, and dry the solid at 40°C to obtain 34.6 g of white solid powder of ceftiofur hydrochloride, with...

Embodiment 3

[0033] The synthesis of embodiment 3 ceftiofur hydrochloride

[0034] Add 40 g of cefuroxime and 240 mL of dichloromethane into a 1000 mL three-necked reaction flask, cool the mixture to 10°C, add 25.4 g of diethylamine dropwise, finish adding dropwise in 20 minutes, and add AE-Active in batches after stirring for 20 minutes Add 12 mL of water to 61.7 g of ester, keep stirring at 10°C for 3 hours, extract twice with 250 mL of water, combine the water phases, add 8 g of activated carbon to decolorize for 30 min, filter, add 28 mL of 5 mol / L hydrochloric acid to the filtrate to adjust the pH value 1.7, filter to obtain a solid wet product, dissolve it in 320 mL of acetone, add 18 mL of 5 mol / L hydrochloric acid dropwise under stirring to adjust the pH value to 1.4, slowly add 2560 mL of water dropwise, gradually a solid precipitates out, stir for 30 min, Let stand for 2 h, filter, and dry the solid at 40°C to obtain 48.3 g of white solid powder of ceftiofur hydrochloride, with a...

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Abstract

The invention relates to preparation of a veterinary use chemical raw medicine and specifically relates to a preparation method of ceftiofur hydrochloride. Ceftiofur acid and AE active ester are used to synthetize ceftiofur in an organic solvent under the action of organic amine, a reaction liquid is extracted by water, hydrochloric acid is added after an aqueous phase extract liquid is decolorized to adjust potential of hydrogen (pH) to be 1-2, solid is separated out and filtered, a wet product is dissolved by an appropriate amount of acetone, water is slowly and dropwise added to elute crystals, filtering is performed, and the solid is dried to obtain the ceftiofur hydrochloride. According to the preparation method of the ceftiofur hydrochloride, the water is used as a crystallization solvent so that the organic solvent is reduced, reducing of production costs is facilitated, and environment pollution is reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis of veterinary raw materials, in particular to a preparation method of ceftiofur hydrochloride. Background technique [0002] Ceftiofur (ceftiofur) is the first third-generation cephalosporin antibiotic dedicated to livestock and poultry. It has a broad-spectrum bactericidal effect and is effective against Gram-positive and negative bacteria, including beta-lactamase-producing strains. Sensitive bacteria include Actinobacillus, Salmonella, Streptococcus, Staphylococcus and so on. The antibacterial activity is stronger than ampicillin, and the activity against streptococci is also stronger than quinolone antibacterial drugs. Its structure has a lactam ring and a furan chain. After entering the body, the furan chain is first degraded to produce a metabolite - desfuran ceftiofur. Due to the integrity of the lactam ring, it still has a strong bactericidal effect, so ceftiofur itself is It has long-a...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04
Inventor 朱振刚夏雪林刘拓
Owner RINGPU TIANJIN BIOLOGICAL PHARMA
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