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Preparation method of cefoperazone sodium

A technology of cefoperazone sodium and cefoperazone acid, which is applied in the field of medicine, can solve the problems of solvents and residues that cannot be effectively solved, and achieve the effects of low acetone solvent residues, uniform particles, and simple operation

Active Publication Date: 2021-01-29
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Patent CN106432273A discloses a method for preparing cefoperazone sodium compound and its preparation using the principle of hydrodynamics. The problem of solvent residue in the product cannot be effectively solved by adding acetone for crystallization

Method used

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  • Preparation method of cefoperazone sodium
  • Preparation method of cefoperazone sodium
  • Preparation method of cefoperazone sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 50ml of acetone to the reaction tank, lower the temperature to 0°C, add 50g of cefoperazone acid, stir and control the temperature at 0°C; add 10ml of purified water to another dissolving tank, control the temperature at 60°C, add 6.5g of sodium bicarbonate, stir to dissolve Clear; add the lye stream to the cefoperazone acid solution, control the temperature at 0°C, and press it into the crystallization tank through the sterilizing filter line after the stream is added;

[0034] Pass sterile nitrogen and acetone into the crystallization tank through the gas-liquid two-phase nozzle, keep the acetone flow rate at 3ml / min, and the nitrogen pressure at 5MPa; when the acetone flow reaches 250ml, add 0.5g of seed crystal and grow the crystal for 15min; Add nitrogen and acetone to the liquid two-phase nozzle to keep the flow rate and pressure constant; after adding acetone to 750ml, cool down and grow the crystal.

[0035] Filtration, vacuum drying, discharging, obtain cef...

Embodiment 2

[0037] Add 75ml of acetone to the reaction tank, lower the temperature by 10°C, add 50g of cefoperazone acid, stir and control the temperature at 10°C; add 13ml of purified water to another dissolution tank, control the temperature at 70°C, add 7.1g of sodium bicarbonate, stir to Clear; add the lye stream to the cefoperazone acid solution, control the temperature at 10°C, and press it into the crystallization tank through the sterilizing filter line after the stream is added;

[0038] Pass sterile nitrogen and acetone into the crystallization tank through the gas-liquid two-phase nozzle, keep the acetone flow rate at 5ml / min, and the nitrogen pressure at 5MPa; Add nitrogen and acetone to the liquid two-phase nozzle to keep the flow rate and pressure constant; after adding acetone to 100ml, cool down and grow the crystal.

[0039] Filtrate, vacuum dry, and discharge to obtain 47.7 g of cefoperazone sodium product.

Embodiment 3

[0041] Add 65ml of acetone to the reaction tank, lower the temperature by 5°C, add 50g of cefoperazone acid, stir and control the temperature at 5°C; add 11ml of purified water to another dissolution tank, control the temperature at 65°C, add 6.8g of sodium bicarbonate, stir to Clear; add the lye stream to the cefoperazone acid solution, control the temperature at 5°C, and then press it into the crystallization tank through the sterilizing filter line after the stream is added;

[0042] Pass sterile nitrogen and acetone into the crystallization tank through the gas-liquid two-phase nozzle, keep the acetone flow rate at 4ml / min, and the nitrogen pressure at 5MPa; Add nitrogen and acetone to the liquid two-phase nozzle to keep the flow rate and pressure constant; after adding acetone to 850ml, cool down and grow the crystal.

[0043] Filtrate, vacuum dry, and discharge to obtain 47.2 g of cefoperazone sodium product.

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Abstract

The invention discloses a preparation method of cefoperazone sodium, which comprises the steps of S1, adding acetone into a reaction tank, stirring to control the temperature, and adding cefoperazoneacid to obtain a cefoperazone acid solution; S2, adding purified water and sodium bicarbonate into a dissolving tank, stirring and controlling the temperature to obtain alkali liquor; S3, feeding thealkali liquor in the step S2 into a cefoperazone acid solution, controlling the temperature, and pressing into a crystallizing tank through a degerming and filtering line; S4, respectively introducingsterile nitrogen and acetone into the crystallizing tank through a gas-liquid two-phase nozzle; S5, adding seed crystal, stirring and growing crystal; S6, continuously adding nitrogen and acetone through the gas-liquid two-phase nozzle; and S7, after feeding is completed, conducting cooling, crystal growing, filtering, vacuum drying and discharging. The cefoperazone sodium powder prepared throughthe method is uniform in particle, small in specific volume and low in acetone solvent residue.

Description

technical field [0001] The invention relates to a preparation method of cefoperazone sodium, which belongs to the technical field of medicine. Background technique [0002] The chemical name of cefoperazone sodium is (6R,7R)-3-[[(1-methyl-1H-tetrazol-5-yl)sulfur]methyl]-7-[(R)-2-(4-ethyl- 2,3-Dioxo-1-piperazinecarbonylamino)-2-p-hydroxyphenyl-acetylamino]-8-oxo-5-thia-1-azabicyclo[4.2.0]octane- 2-ene-2-carboxylic acid sodium salt, white to light yellow powder or crystalline powder, easily soluble in water, slightly soluble in methanol, very slightly soluble in ethanol, insoluble in acetone or ethyl acetate, its structural formula is as follows: [0003] [0004] The preparation method of cefoperazone sodium mainly contains two kinds of methods, and a kind of is solvent crystallization method, and a kind of is freeze-drying crystallization method. Freeze-drying crystallization method obtains an amorphous substance, and impurities are wrapped in the product, resulting in ...

Claims

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Application Information

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IPC IPC(8): C07D501/04C07D501/12C07D501/36
CPCC07D501/04C07D501/12C07D501/36
Inventor 任峰贾全田洪年张建丽魏宝军刘树斌杨梦德贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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