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Method for preparing cefoperazone sodium

A technology of cefoperazone sodium and cefoperazone acid, which is applied in the field of medicine, can solve the problems of high acetone residue, achieve drug safety, shorten the production cycle, and improve product quality and stability

Active Publication Date: 2016-03-30
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved in the present invention is to provide a method for preparing cefoperazone sodium, which solves the problem of high residual acetone in the prior art, improves product quality and stability, and makes medication safer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A. Dissolution: Add 500L of acetone and 100L of purified water to the reaction tank, start stirring, then add 100kg of cefoperazone acid, control the temperature at 20±10°C, add saturated sodium bicarbonate solution to adjust the pH to 6.8, and dissolve the cefoperazone acid completely.

[0040] B. Decolorization: Add 5kg of medicinal active carbon to the solution in step A for decolorization, then pass through the decarburization filter and the multi-stage sterilizing filter element successively, and press into the crystallization tank in the aseptic room.

[0041] C. Crystallization: The crystallization tank was turned on and stirred, and 1500L of acetone was added to the crystallization tank to crystallize; the crystal was grown under stirring for 0.5h, filtered with a three-in-one filter, and the filter cake was washed with acetone.

[0042] D. Drying: The washed filter cake enters the drying equipment with a direct-ray atomization device installed on the top, atom...

Embodiment 2

[0044]A. Dissolution: Add 450L of acetone and 100L of purified water into the reaction tank, start stirring, then add 100kg of cefoperazone acid, control the temperature at 20±10°C, add 150L of saturated sodium acetate solution dropwise, adjust the pH to 7.6, and dissolve the cefoperazone acid Dissolve completely.

[0045] B. Decolorization: Add 5kg of medicinal active carbon to the solution in step A for decolorization, then pass through the decarburization filter and the multi-stage sterilizing filter element successively, and press into the crystallization tank in the aseptic room.

[0046] C. Crystallization: The crystallization tank was turned on and stirred, and 40L of ethanol and 1500L of acetone were poured into the crystallization tank to crystallize; the crystal was grown for 1 hour under stirring, filtered with a three-in-one filter, and the filter cake was washed with acetone.

[0047] D. Drying: The washed filter cake enters the drying equipment with a direct-ray...

Embodiment 3

[0049] A. Dissolution: Add 350L of acetone and 100L of purified water into the reaction tank, start stirring, then add 100kg of cefoperazone acid, control the temperature at 20±10°C, add saturated sodium carbonate solution dropwise to adjust the pH to 7.0, and dissolve the cefoperazone acid completely .

[0050] B. Decolorization: Add 5kg of medicinal active carbon to the solution in step A for decolorization, then pass through the decarburization filter and the multi-stage sterilizing filter element successively, and press into the crystallization tank in the aseptic room.

[0051] C. Crystallization: The crystallization tank was turned on and stirred, and 80L of isopropanol and 1500L of acetone were added into the crystallization tank to crystallize; the crystal was grown under stirring for 1.5h, filtered with a three-in-one filter, and the filter cake was washed with acetone.

[0052] D. Drying: The washed filter cake enters the drying equipment with a direct-ray atomizati...

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PUM

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Abstract

The invention discloses a method for preparing cefoperazone sodium. The method comprises steps as follows: dissolving: acetone and purified water are added to a reaction tank, stirring is started, cefoperazone acid is added, pH (potential of hydrogen) is adjusted to be 6.8-7.2, and cefoperazone acid is completely dissolved; decoloration: activated carbon is added to a cefoperazone acid solution for decoloration, and the cefoperazone acid solution is pressed into a crystallizing tank of a sterilizing room through a decarbonization filter and a multilevel bacterium removal filter element; crystallization: an organic solvent is fed to the crystallizing tank for crystallization; crystals grow under the stirring condition, a three-in-one filter is used for filtration, and a filter cake is washed with acetone; drying: the washed filter cake enters a drying device, sterilized and filtered methanol, water or methanol water is atomized through a direct-injection type atomization device, atomized steam is driven by sterile nitrogen to blow the filter cake for 2 h plus or minus 1.5 h, then, hot water is provided for circulation heating, the filter cake is dried in a vacuum state until residual solvents are qualified, and then cefoperazone sodium is discharged. The acetone residues in a cefoperazone sodium product are far smaller than 0.5%, the product quality and the stability are improved, medication is safer, and good social benefits are generated.

Description

technical field [0001] The invention belongs to the technical field of medicine, in particular to a method for preparing cefoperazone sodium. Background technique [0002] Cefoperazone sodium (Cefoperazonesodium, CAS number: 62893-20-3), its chemical name is: (6R,7R)-3-[[(1-methyl-1H-tetrazol-5-yl)thio]methyl]- 7-[(R)-2-(4-Ethyl-2,3-dioxo-1-piperazinecarbonylamino)-2-p-hydroxyphenyl-acetylamino]-8-oxo-5- Thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt is a third-generation broad-spectrum, long-acting cephalosporin antibiotic, which produces antibacterial activity by inhibiting bacterial cell wall synthesis, and is used for sensitive The treatment of various infections caused by enzyme-producing bacteria, such as the treatment of respiratory system, genitourinary system, biliary tract, gastrointestinal tract, chest and abdominal cavity, skin and soft tissue infections, and also has a good effect on intracerebral infections caused by influenza bacillus and men...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04C07D501/12
CPCC07B2200/13C07D501/04C07D501/12C07D501/36
Inventor 胡利敏魏青杰谭清钟张锁庆李惠芬倪福震左梦祥任峰刘树斌郭玉聪杨梦思
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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