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Method for preparing anhydrous beta-aztreonam

A technology of aztreonam and organic solvents, applied in the field of refining β-aztreonam and high-purity β-aztreonam, which can solve problems such as major technical defects or hidden quality problems, unfeasible production, unfavorable industrial production, etc.

Active Publication Date: 2012-01-11
HAINAN HAIYAO CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the above methods all have relatively large technical defects or hidden dangers in quality.
The method recorded in the U.S. patent application US946838 uses high-temperature heating to dissolve, which will destroy the structure of the product and easily cause its decomposition. Second, even if it is temporarily dissolved, the time is short and it cannot pass sterile filtration. It is unfeasible in production.
The current general amine-HCl-ethanol preparation method, due to the strong corrosiveness of hydrochloric acid gas, especially the corrosiveness of chloride ions, puts forward higher requirements for aseptic equipment, and at the same time, the long-term erosion of chloride ions has a negative effect on the anti-corrosion of clean areas and equipment materials. All have different degrees of damage, and there are greater equipment hidden dangers and quality risks
The method of dissolving with a large-scale solvent is the same as dissolving at a high temperature, which is not conducive to industrial production. The dissolution of a mixed solvent also requires a large-scale solvent, and the mixed solvent is not easy to recycle and apply mechanically.

Method used

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  • Method for preparing anhydrous beta-aztreonam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Add 500ml of absolute ethanol to a three-necked bottle, add 40g of α-aztreonam with a water content of 11%, stir, add 10ml of triethylamine at 25°C, add 4g of activated carbon after it is completely dissolved, and decolorize at room temperature for 30min. Filter and add the filtrate to a 1000ml crystallization tank;

[0027] 2) Take another 100ml round bottom flask, add 50ml of 30% ethanol anhydrous formic acid, add 0.5g of activated carbon, decolorize at room temperature for 30min, filter with a stainless steel sterilizing filter, add the mother liquor dropwise to the crystallization tank of step 1), and adjust the pH value 2.5, stirred to precipitate crystals, grown the crystals for 2 hours, filtered, washed with 100ml of acetone, and dried to obtain 31.5g of β-aztreonam fine product, with a yield of 78.75%, a water content of 1.2%, and a content of 98.8%.

Embodiment 2

[0029] 1) Add 500ml of absolute ethanol to a three-necked bottle, add 40g of α-aztreonam with a water content of 11%, stir, add 10ml of triethylamine at 25°C, add 4g of activated carbon after it is completely dissolved, and decolorize at room temperature for 30min. Filter and add the filtrate to a 1000ml crystallization tank;

[0030] 2) Take another 100ml round bottom flask, add 50ml of 30% anhydrous oxalic acid ethanol, add 0.5g of activated carbon, decolorize at room temperature for 30min, filter with a stainless steel sterilizing filter, add the mother liquor dropwise to the crystallization tank of step 1), adjust The pH value was 2, crystals were precipitated by stirring, grown for 2 hours, filtered, washed with 100ml of acetone, and dried to obtain 33.5g of β-aztreonam fine product, with a yield of 83.75%, a water content of 1.2%, and a content of 98.71%.

Embodiment 3

[0032]1) Add 500ml of absolute ethanol to a three-necked bottle, add 40g of α-aztreonam with a water content of 11%, stir, add 10ml of triethylamine at 25°C, add 4g of activated carbon after it is completely dissolved, and decolorize at room temperature for 30min. Filter, and add the filtrate to a 1000ml crystallization tank;

[0033] 2) Take another 100ml round bottom flask, add 50ml of 30% ethanol anhydrous benzoate, add 0.5g of activated carbon, decolorize at room temperature for 30min, filter with a stainless steel sterilizing filter, add the mother liquor dropwise to the crystallization tank of step 1), and adjust the pH When the value was 2, crystals were precipitated by stirring, grown for 2 hours, filtered, washed with 100ml of acetone, and dried to obtain 33.8g of β-aztreonam, with a yield of 84.5%, a water content of 1.12%, and a content of 98.5%.

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Abstract

The invention provides a method for preparing anhydrous beta-aztreonam. Based on preparation methods of amine-HCl-ethanol in the prior art, the method provided by the invention comprises steps of replacing inorganic acid with organic acid, carrying out neutralization, cooling and crystallizing, thus avoiding the corrosion of inorganic acid to equipment in clean areas and latent quality risk, guaranteeing the quality stability of the product and making the production to keep running normally.

Description

technical field [0001] The invention relates to a method for refining beta-aztreonam, in particular to a method for preparing high-purity beta-aztreonam from alpha-aztreonam, which belongs to the field of medicine and chemical industry. Background technique [0002] Aztreonam is the first clinically synthesized monocyclic lactam antibiotic developed by Bristol-Myers Squibb Company in the United States. It was launched in Pakistan in 1986 and listed in Indonesia under the trade name Azactam in 1988. It was listed in Japan in 1987, and it was also listed in Germany, Spain, France, etc. The raw materials were imported to China in 2002, and the preparation was produced and launched in my country by Bristol-Myers Squibb in 1997. Aztreonam has a high degree of antibacterial activity against most aerobic Gram-negative bacteria, including Escherichia coli, Klebsiella pneumoniae and Oxytobacter, aerogenes, cloacae, Proteus, sand Enterobacteriaceae such as Rhysporum, Citrobacter, an...

Claims

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Application Information

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IPC IPC(8): C07D417/12
Inventor 白智全吴建军孙文魁张志兰沙莹
Owner HAINAN HAIYAO CO LTD
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