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Cefepime halogen acid salt preparation method

A technology of hydrohalide salts and cefepime, which is applied in the field of preparation of cephalosporin compounds, can solve problems such as reducing production costs, and achieve the effects of reducing production costs, improving purity, and saving production costs

Active Publication Date: 2009-02-04
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 the present invention is to provide a new method for preparing cefepime hydrohalide salt by cefepime sulfate, which solves the problem of hydrogen halide corrosion crystallization equipment in the synthesis process of cefepime hydrohalide salt, and greatly reduces production capacity. cost, while improving the purity of cefepime hydrohalide

Method used

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Examples

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Effect test

Embodiment 1

[0032] Dissolve 8g of barium chloride dihydrate (32.8mmol, which is 0.95 times the molar ratio of cefepime sulfate) in 70mL of water at room temperature, and then add 20g of cefepime sulfate (34.5mmol, weight by anhydrous ) to form a slurry system with good fluidity. After 10 minutes, add an 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 water, and combine the filtrates. 600 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 18 g of white crystalline powder. The purity is 99.7% (HPLC), the water content is 4.0% (K-F method), the residual acetone is 0.31% (gas chromatography), and the pH of the...

Embodiment 2

[0034]Dissolve 8g of barium chloride dihydrate (32.8mmol) in 60mL of water at room temperature, and then add 20g of cefepime sulfate (34.5mmol, weight based on anhydrous matter) in batches under effective stirring to form a slurry system with good fluidity . After 10 minutes, add an appropriate amount of activated carbon and 30 mL of methanol, and stir for 30 minutes. The solid was isolated by centrifugation or suction filtration. Wash the filter cake with an appropriate amount of methanol-water 1:1 (v / v) mixed solution, and combine the filtrates. 600 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 17.5 g of white crystalline powder. The water content is 3.8% (K-F method), the remaining acetone is 0.35%, and the remaini...

Embodiment 3

[0036] Dissolve 8g of barium chloride dihydrate (32.8mmol) in 60mL of water at room temperature, and then add 30mL of methanol. Under effective stirring, 20 g of cefepime sulfate (34.5 mmol, calculated as anhydrous matter) was added in batches to form a slurry system with good fluidity. After stirring for 30 minutes, the solid was separated by centrifugation or suction filtration. Wash the filter cake with an appropriate amount of methanol-water 1:1 (v / v) mixed solution, and combine the filtrates. 600 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 17.5 g of white crystalline powder. Content and water content data show that the product is also cefepime dihydrochloride monohydrate. Acetone remained 0.30%, methanol remain...

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Abstract

The invention relates to a method for preparing cefepime hydrohaloride. It takes sulfate of cefepime as raw material and produce cefepime hydrohaloride with barium halide. It effectively solves the corrosive problem to producing device, reduces production cost and increases product purity.

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 barium halide as raw materials. [Background technique] [0002] Cefepime (cefepime) is the fourth-generation cephalosporin antibiotics for injection, developed by the American Boomer-Squibb (BMS) company (US 4,406,899), and was first listed in Sweden in 1993. It entered my country in 1998 with the product name "Masipime". 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. [0003] Cefepime is a neutral inner salt wit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/56
Inventor 谭端明叶澄海
Owner SHENZHEN SALUBRIS PHARMA CO LTD
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