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Preparation of cefepime halogen acid salt by calcium salt precipitation process

A technology of hydrohalide salt and cefepime, which is applied in the field of preparation of cephalosporins, can solve problems such as pollution, and achieve the effects of reducing emissions, saving production costs and prolonging service life

Inactive Publication Date: 2007-09-26
SHENZHEN SALUBRIS PHARMA CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of this invention is to provide a new salt conversion method to convert cefepime sulfate into cefepime hydrohalide, which not only solves the pollution caused by the use of freon in the production process, or avoids the pollution caused by the use of solid resin. material waste, and also improved the yield of cefepime hydrohalide

Method used

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  • Preparation of cefepime halogen acid salt by calcium salt precipitation process

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Experimental program
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Effect test

Embodiment 1

[0033]Dissolve 10.5g of calcium chloride dihydrate (71mmol, 0.9 times the molar ratio of cefepime sulfate) in 110mL of water at room temperature, and then add 40g of cefepime sulfate (79mmol, weight based on anhydrous matter) in batches under effective stirring. ), forming a slurry system with good fluidity. After 10 minutes, add 180 mL of acetone and appropriate amount of activated carbon, and stir for 30 minutes. The solid was isolated by centrifugation or suction filtration. Wash the filter cake with an appropriate amount of acetone-water 2:1 (v / v) mixed solution, and combine the filtrates. 1200 mL of acetone was added to the filtrate under stirring, and the addition was completed within about 1 hour. The temperature of the system was lowered to 0-5°C again, and the stirring was continued for 1 hour. Suction. The filter cake was washed with acetone and dried under vacuum at 40°C to obtain about 35.2 g of white crystalline powder. The water content is 3.7% (K-F method),...

Embodiment 2

[0035] Dissolve 12.8g of calcium chloride dihydrate (87mmol, 1.1 times the molar ratio of cefepime sulfate) in 110mL of water at room temperature, and then add 40g of cefepime sulfate (79mmol, weight based on anhydrous matter) in batches under effective stirring. ), forming a slurry system with good fluidity. After 10 minutes, add 180 mL of acetone and appropriate amount of activated carbon, and stir for 30 minutes. The solid was isolated by centrifugation or suction filtration. Wash the filter cake with an appropriate amount of acetone-water 2:1 (v / v) mixed solution, and combine the filtrates. 1200 mL of acetone was added to the filtrate under stirring, and the addition was completed within about 1 hour. The temperature of the system was lowered to 0-5°C again, and the stirring was continued for 1 hour. Suction. The filter cake was washed with acetone and dried under vacuum at 40° C. to obtain about 36 g of white crystalline powder. The product is cefepime dihydrochlorid...

Embodiment 3

[0037] Dissolve 11.6g of calcium chloride dihydrate (79mmol, 1.0 times the molar ratio of cefepime sulfate) in 90mL of water and 20mL of methanol at normal temperature, then add 40g of cefepime sulfate (79mmol, weight according to water content), forming a slurry system with good fluidity. After 10 minutes, 90 mL of methanol and an appropriate amount of activated carbon were added, and stirred for 30 minutes. The solid was isolated by centrifugation or suction filtration. Wash the filter cake with an appropriate amount of acetone-water 2:1 (v / v) mixed solution, and combine the filtrates. 1500 mL of acetone was added to the filtrate under stirring, and the addition was completed within about 1 hour. The temperature of the system was lowered to 0-5°C again, and the stirring was continued for 1 hour. Suction. The filter cake was washed with acetone and dried under vacuum at 40° C. to obtain about 34.8 g of white crystalline powder. The product is cefepime dihydrochloride mon...

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Abstract

The invention discloses a making method of cefazedone halogen acid salt, which is characterized by the following: adopting sulfate of cefazedone as raw material; reacting with calcium halide; improving the receiving rate with less environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of cephalosporin compounds, in particular to a method for preparing cefepime hydrohalide by using cefepime sulfate and calcium halide as raw materials. Background technique [0002] Cefepime (cefepime) is the fourth-generation cephalosporin injectable antibiotic (US 4,406,899) developed by American Boomer-Bristol-Myers Squibb (BMS), which was first listed in Sweden in 1993. Cefepime has good antibacterial activity against Gram-negative bacteria (such as Enterobacter, Pseudomonas aeruginosa), Gram-positive bacteria (such as Streptococcus pneumoniae, Staphylococcus aureus) and anaerobic bacteria, and has good antibacterial activity against β- Lactamase exhibits higher stability, and has a wider antibacterial spectrum and antibacterial activity than the third-generation cephalosporin antibiotics. It is clinically used to treat severe infections. [0003] Cefepime is a neutral inner salt with high water solub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46
Inventor 谭端明叶澄海
Owner SHENZHEN SALUBRIS PHARMA CO LTD
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