Purification method of cefpiramide acid

A technology of cefpiramide and a refining method, which is applied in the refining field of cefpiramide, can solve the problems of poor yield and low purity of cefpiramide, and achieves low production cost, high yield, and simple operation in the preparation process. Effect

Active Publication Date: 2020-04-28
湖北凌晟药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problems of low purity and poor yield of existing cefpiramic acid, the invention provides a method for refining cefpiramic acid

Method used

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  • Purification method of cefpiramide acid

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Effect test

Embodiment 1

[0029] The present embodiment provides a kind of refining method of cefpiramide, comprising the following steps:

[0030] Step a, add 340L methanol and 80Kg cefpiram acid crude product (TPC) to R-125 reaction kettle, drop triethylamine 20.96Kg under the condition of 10 ℃, dropwise time is 30min, obtains cefpiram acid three Ethylamine salt solution;

[0031] Step b, add 1200L of acetone to the cefpiramide salt solution at 20°C, stir at a speed of 300rpm for 1h, then cool down to 10°C for centrifugal filtration at a speed of 800rpm, and wash with 150L of acetone, Dried time is 30min, obtains cefpiramic acid triethylamine salt (TPT);

[0032] Step c, add 600L of purified water to the R-225 reactor, and add the cefpiramic acid triethylamine salt obtained in step b, mix at 10°C for 10min, then raise the temperature to 15°C and add 5Kg of activated carbon for decolorization for 20min, Filter to remove carbon, collect the filtrate into the crystallization tank R-325, and add 2M hyd...

Embodiment 2

[0034] The present embodiment provides a kind of refining method of cefpiramide, comprising the following steps:

[0035] Step a, add 160L ethanol and 80Kg cefpiramic acid crude product (TPC) in R-125 reactor, drop triethylamine 22.1Kg under the condition of 12 ℃, dropwise time is 25min, obtains cefpiramic acid three Ethylamine salt solution;

[0036] Step b. Add 960L of isopropanol to the cefpiramide salt solution at 18°C, stir for 70min at a speed of 200rpm, then cool down to 15°C for centrifugal filtration at a speed of 700rpm, using 160L isopropanol Propanol washing, drying time is 60min, to obtain cefpiramide triethylamine salt (TPT);

[0037] Step c, add 640L of purified water to the R-225 reaction kettle, and add the cefpiramic acid triethylamine salt obtained in step b, mix at 12°C for 8 minutes, then raise the temperature to 18°C ​​and add 4Kg of activated carbon for decolorization for 25 minutes, Filter to remove carbon, collect the filtrate into the crystallizatio...

Embodiment 3

[0039] The present embodiment provides a kind of refining method of cefpiramide, comprising the following steps:

[0040] Step a, add 200L methanol and 80Kg cefpiram acid crude product (TPC) to the R-125 reaction kettle, add 17.8Kg of triethylamine dropwise under the condition of 13°C, and the dropping time is 32min to obtain cefpiramic acid tri Ethylamine salt solution;

[0041] Step b, add 1360L propylene glycol to the cefpiramide salt solution at 22°C, stir at a speed of 250rpm for 50min, then cool down to 12°C for centrifugal filtration at 750rpm, wash with 120L propylene glycol, The spin-drying time is 40min to obtain cefpiramic acid triethylamine salt (TPT);

[0042] Step c. Add 560L of purified water to the R-225 reactor, and add the cefpiramic acid triethylamine salt obtained in step b, mix at 15°C for 10 minutes, then raise the temperature to 20°C and add 5.6Kg of activated carbon for decolorization for 30 minutes , filter to remove carbon, collect the filtrate into...

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Abstract

The invention relates to the technical field of medicine purification, and particularly discloses a purification method of cefpiramide acid. The method comprises the following steps: mixing an alcoholsolvent with a cefpiramic acid crude product, and then adding triethylamine to obtain a cefpiramic acid triethylamine salt dissolving solution; adding a precipitant into the cefpiramide acid amine salt dissolving solution, mixing, stirring, centrifugally filtering and washing to obtain cefpiramide acid triethylamine salt; and uniformly mixing the cefpiramic acid triethylamine salt with purified water, decolorizing, performing filtration, adjusting the pH value of the collected filtrate to 2-2.5, crystallizing, washing, and carrying out vacuum drying to obtain the refined cefpiramic acid. Therefined cefpiramide acid has the advantages of high purity, high yield, low color grade, simple operation and low production cost, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of medicine purification, in particular to a method for refining cefpiramin. Background technique [0002] Cefpiramide sodium is a cephalosporin for injection jointly developed by Japan's Sumitomo Pharmaceutical Company and Yamanouchi Pharmaceutical Company. According to the age of discovery and antibacterial properties of cephalosporins, it is between the third generation and the fourth generation, so some people simply call it the "third and a half generation" cephalosporins. Cefpiramide sodium was listed in Japan for the first time in 1985. Its structure is characterized by a methyl tetrazolium sulfenyl group at the C3 position, a hydroxyphenyl group and a hydroxymethylpyridyl group at the C7 position, thus greatly improving the efficacy of the original drug. Antibacterial activity and pharmacokinetic profile. [0003] Cefpiramic acid is the precursor raw material of cefpiramide sodium, and its chemical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/12C07D501/36
Inventor 金联明门万辉邹菁
Owner 湖北凌晟药业股份有限公司
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