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Refining method of cefathiamidine

A cefathiamidine and purification method technology, applied in the field of chemical pharmacy, can solve the problems of affecting the yield of cefathiamidine crystals, low purity of cefathiamidine crystals, unable to meet the requirements for use, etc., to improve the effect of dissolution, filtration and decolorization, and the preparation method. Simple and easy to control, the effect of high product yield

Active Publication Date: 2018-12-07
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses an organic solvent to dissolve cefathiamidine, and cefathiamidine itself is easily soluble in water, but its solubility in an organic solvent is not good, so the use of an organic solvent for dissolution is not effective, which affects the yield of cefathiamidine crystals
Only activated carbon is used for decolorization. Although activated carbon has a certain decolorization effect, the color grade of cefathiamidine obtained is still relatively high, and there are many impurities. A high content of impurities will affect the orientation of crystal particles on the crystal surface Arrangement, so that the crystallization proceeds very slowly or even cannot be carried out, and some impurities will form complexes with the crystal particles, and the obtained cefathiamidine crystals have low purity and poor stability, which cannot meet the requirements for use.

Method used

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  • Refining method of cefathiamidine
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  • Refining method of cefathiamidine

Examples

Experimental program
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preparation example Construction

[0034] The preparation method comprises the following steps:

[0035]A. Add 3 to 9 times the dissolving agent of the cefathiamidine crude product quality in the reaction tank, then slowly add the cefathiamidine crude product, stir and dissolve at 0 to 15° C. to dissolve, and obtain the cefathiamidine crude product solution; the dissolving agent is Hydrophilic organic solvent containing water, the content of water in the dissolving agent is 40-80%; the hydrophilic organic solvent is acetone, methyl isobutyl ketone, isopropanol, methanol, ethanol, acetonitrile or 2-butanone any one or a combination of several;

[0036] B. Add 0.05 to 0.3 times of the cefathiamidine crude product quality stabilizer to the cefathiamidine crude product solution, stir evenly, then add 5 to 10% activated carbon of the cefathiamidine crude product quality, filter after stirring, and pass the filtrate into γ-type acidic alumina adsorption column, adjust the flow rate, collect the effluent, then wash t...

Embodiment 1

[0042] A method for refining cefathiamidine comprises the steps of dissolving crude cefathiamidine with a dissolving agent, adding a stabilizing regulator, and performing secondary decolorization by using an alumina adsorption column.

[0043] The preparation method comprises the following steps:

[0044] A. Add 40 mL of acetone containing 40% water in the reaction tank, and the dissolution temperature is 5° C., slowly add 10 g of cefathiamidine crude product, stir until dissolved, and obtain cefathiamidine crude product solution;

[0045] B. Add 0.5 mL of potassium dihydrogen phosphate and sodium hydroxide buffer solution with pH 5.0 to the crude cefathiamidine solution, stir evenly, then add 0.5 g of activated carbon, stir for 1 hour, filter, and pass the filtrate into γ-type acidic alumina For the adsorption column, adjust the flow rate to 2 mL / min, collect the effluent, then wash the alumina adsorption column with a dissolving agent, then wash with 4 mL of acetone containi...

Embodiment 7

[0053] This example is a comparative example. Prepare cefathiamidine according to the method described in the patent document CN102532165A. At -2°C, dissolve 20 g of cefathiamidine crude product in 180 mL of anhydrous methanol and 150 mL of anhydrous isopropanol, add 20 g of molecular sieves and 2 g of activated carbon after dissolution, and stir for dehydration , decolorize for 20min, filter, stir 60r / min, add 600mL of anhydrous isopropanol to the filtrate, add 4.5h, filter, wash twice with 80mL of anhydrous isopropanol, wash three times with 120mL of anhydrous acetone, 35 Cefathiamidine was dried under vacuum for 28 hours to obtain 15.13 g of cefathiamidine.

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Abstract

The invention discloses a refining method of cefathiamidine, belonging to the chemical pharmacy field. The refining method comprises the steps of dissolving a cefathiamidine crude product by virtue ofa dissolving agent, adding a stable adjusting agent, and carrying out secondary decolorization by virtue of an aluminum oxide adsorption column. According to the refining method, the color grade of cefathiamidine can be effectively decreased, obtained cefathiamidine crystal particles are uniform, high in purity and good in stability, the product yield is high, and the preparation method is easy,convenient and controllable and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for refining a compound, in particular to a method for refining a β-lactam antibiotic, and belongs to the field of chemical pharmacy. Background technique [0002] Cefathiamidine is a β-lactam antibiotic and belongs to the first generation of cephalosporins for injection. Its chemical name is (6R,7R)-3[(acetoxy)methyl]-7-[α-(N, N-Diisopropylamidinothio)acetamido]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate betaine, the molecular formula is C 19 h 28 N 4 o 6 S 2 , the structural formula is: [0003] [0004] Cefathiamidine is a broad-spectrum antibiotic with good antibacterial activity against Gram-positive bacteria and some negative bacilli, especially Staphylococcus aureus, Staphylococcus epidermidis, Streptococcus pneumoniae, Enterococcus (including drug-resistant strains ) and other Gram-positive cocci. Widely used in respiratory tract infection, trauma and surgical infection, skin and soft tis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/28C07D501/12
CPCC07D501/12C07D501/28
Inventor 李庆伟石春利张锁庆任峰贾全田洪年刘树斌于亚南宋玮
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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