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Method for producing beta crystal system anhydrous aztreonam

A technology of aztreonam and β crystal form, which is applied in the production field of β crystal form anhydrous aztreonam, can solve the problems of large amount of absolute ethanol, low industrial production efficiency, and high ethanol content of β crystal form aztreonam, Achieve the effects of reducing ethanol content, improving production efficiency and simplifying the production process

Inactive Publication Date: 2008-06-11
BEIJING GUANGFENG XIANFENG BIOTECH
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Problems solved by technology

However, the yield of this method is very low
[0009] Chinese patent CN1545514A discloses a method for preparing sterile anhydrous β crystal form aztreonam, which dissolves α crystal form aztreonam in absolute ethanol at a lower temperature, then sterilizes and filters, reheats and Stir to obtain the solution, and the β crystal form aztreonam is separated out from the solution. The main disadvantage of this method is that the amount of dehydrated alcohol used to dissolve the α crystal form aztreonam is very large (60 times), so the industrial production efficiency is low
Another shortcoming is that the obtained β crystal form aztreonam contains higher ethanol (about 2.4%), which is not suitable for medicinal use

Method used

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  • Method for producing beta crystal system anhydrous aztreonam

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reference example 1

[0026] At 8-10°C, add α-crystalline aztreonam (40g) into pre-cooled absolute ethanol (2400ml), stir for 30 minutes to obtain a transparent solution, keep at 8-10°C, add activated carbon (1g) and stir the above solution for 15 minutes, the resulting suspension was filtered, and the filter cake was washed with ethanol (50ml). Afterwards, the filtrate was slowly heated to 50-55°C within 2 hours under stirring, and crystals were precipitated as β crystal form aztreonam. The liquid was cooled to 15-20°C, stirred for 1 hour and filtered again, and the resulting crystalline product was dried in vacuo to obtain 28 g of product. Infrared spectra and powder X-ray diffraction showed that the crystal form of the product was consistent with that of the standard product (β crystal form aztreonam). Gas chromatographic analysis showed that the ethanol content was 2.3%.

Embodiment 1

[0028] At 10-15°C, add α crystal form aztreonam (40g) into pre-cooled absolute ethanol and acetone (3∶1) (1000ml), stirred for 5 minutes to obtain a transparent solution, kept at 10-15°C, added activated carbon (1g) and stirred the above solution for 15 minutes, filtered the resulting suspension, washed the filter cake with acetone (50ml), and then stirred The lower filtrate was slowly heated to 35-40° C. within 2 hours, and the precipitated crystals were β crystal form aztreonam. The suspension was cooled to 15-20°C, stirred for 1 hour and filtered again, and the resulting crystalline product was dried in vacuo to yield 33.5 g of product. Infrared spectra and powder X-ray diffraction showed that the crystal form of the product was consistent with that of the standard product (β crystal form aztreonam). Gas chromatographic analysis showed that the ethanol content was 0.9%.

Embodiment 2

[0030] At 10-15°C, add α crystal form aztreonam (40g) into pre-cooled absolute ethanol and acetone (3∶1) (1000ml), stirred for 5 minutes to obtain a transparent solution, kept at 10-15°C, added activated carbon (1g) and stirred the above solution for 15 minutes, filtered the resulting suspension, washed the filter cake with acetone (50ml), and filtered out After the solution was vigorously stirred for 40 minutes, white crystals began to precipitate. Continue to stir for 1 hour, and a large amount of crystals precipitated. Under stirring, the solution was slowly heated to 35-40°C within 30 minutes to completely precipitate the crystals. The precipitated crystals were β crystal form aztreonam . The suspension was cooled to 15-20°C, stirred for 1 hour and filtered again, and the resulting crystalline product was dried in vacuo to yield 32 g of product. Gas chromatographic analysis showed that the ethanol content was 0.4%.

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Abstract

The invention relates to a production method of anhydrous beta-type aztreonam, which comprises dissolving alpha-crystal-system aztreonam in the mixture of absolute ethyl alcohol and acetone at -10-+25DEG C, filtering without germ, heating the solution to 30-55DEG C, or seriously mixing to obtain anhydrous beta-type aztreonam crystals.

Description

technical field [0001] The invention relates to a production method of anhydrous β crystal form aztreonam crystal. Background technique [0002] Aztreonam (Aztreonam) shown in molecular formula I is a synthetic monocyclic β-lactam antibiotic, which has antibacterial activity against Gram-negative bacteria. [0003] [0004] Molecular formula I [0005] Some references report the preparation technology of aztreonam, for example: US Patent Nos. 4,775,670 and 5,194,604. Aztreonam has polymorphism, and US Pat. No. 4,826,973 reports four different crystals of aztreonam, namely α-, β-, γ-, and δ-types. The α crystal form is a hydrous crystal, usually containing 7-15% water, and has poor stability. Therefore, it should be transformed into the β crystal form, which has the characteristics of anhydrous, non-hygroscopic, good fluidity, smaller surface area, and better stability, and is more suitable for pharmaceutical use. [0006] U.S. Patent No. 4,946,838 reports the preparat...

Claims

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Application Information

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IPC IPC(8): C07D417/12
Inventor 郭庆春刘通
Owner BEIJING GUANGFENG XIANFENG BIOTECH
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