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Preparation method of crystal form B avibactam sodium

A technology of avibactam sodium and crystal form, which is applied in the field of preparation of crystal form B avibactam sodium, and can solve the problems of difficult industrialized and stable production of crystal form B avibactam sodium.

Pending Publication Date: 2021-07-13
SICHUAN KELUN PHARMA RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Based on this, it is necessary to provide a preparation method for crystalline form B avibactam sodium in view of the difficulty in industrialized and stable production of crystalline form B avibactam sodium

Method used

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  • Preparation method of crystal form B avibactam sodium
  • Preparation method of crystal form B avibactam sodium
  • Preparation method of crystal form B avibactam sodium

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preparation example Construction

[0038] The embodiment of the present invention provides a preparation method of crystal form B avibactam sodium, comprising:

[0039] S100, adding methanol and water to the avibactam sodium, then stirring and heating to dissolve to obtain the avibactam sodium solution;

[0040] S200, adding an alcoholic poor solvent into the avibactam sodium solution, cooling to a first temperature, stirring and growing crystals, and then continuing cooling to a second temperature for crystallization.

[0041] The present invention stably prepares crystal form B avibactam sodium by means of crystallization, by adding methanol and water to avibactam sodium, and heating and dissolving to make avibactam sodium of various crystal forms (including amorphous) Transform into a uniform avibactam sodium solution, then add alcohol poor solvents for two-step cooling, first cool down for crystal growth, so that various crystal forms of avibactam sodium can be converted to type B, and then continue to cool...

Embodiment 1

[0062] Step (1): Add 50 mL of methanol and 6 mL of water to 10 g of avibactam sodium in crystal form D in sequence, stir and heat up to 55-60°C to dissolve;

[0063] Step (2): Add 600mL of ethanol dropwise at a stirring speed of 200rpm (, after the dropwise addition is completed, cool down to 30-35°C, continue to grow crystals at a stirring speed of 200rpm for 16h, then cool down to -5-5°C and stir for 2h, filter with suction , washed with 20 mL of ethanol, and dried in vacuum for 14 hours to obtain 8.5 g of avibactam sodium (yield 85%).

[0064] The obtained avibactam sodium sample is analyzed by XRD as anhydrous "B" crystal form avibactam sodium, and the XRD figure is as follows figure 2 shown.

Embodiment 2

[0066] Step (1): Add a mixed solvent of 70 mL of methanol and 5.7 mL of water to 10 g of avibactam sodium in crystal form A, stir and heat up to 60-65°C to dissolve;

[0067] Step (2): Add 530mL of isopropanol dropwise at a stirring speed of 250rpm (, after the dropwise addition is completed, cool down to 25-30°C, continue to grow crystals at a stirring speed of 250rpm for 16h, then cool down to 15-20°C and stir for 1h, pump Filtered, washed with 20 mL of ethanol, and dried in vacuum for 16 hours to obtain 8.0 g of avibactam sodium (yield 80%).

[0068] The obtained avibactam sodium sample is analyzed by XRD as anhydrous "B" crystal form avibactam sodium, and the XRD figure is as follows image 3 shown.

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Abstract

The invention discloses a preparation method of crystal form B avibactam sodium, which comprises the following steps: S100, adding methanol and water into avibactam sodium, stirring, heating and dissolving to obtain an avibactam sodium solution; and S200, adding an alcohol poor solvent into the avibactam sodium solution, cooling to a first temperature, stirring for growing crystals, and then continuously cooling to a second temperature for devitrification.

Description

technical field [0001] The invention relates to the technical field of avibactam sodium production, in particular to a method for preparing crystal form B avibactam sodium. Background technique [0002] Avibactam Sodium (Avibactam Sodium) is a novel non-β-lactam structure β-lactamase inhibitor developed by Novexel. Avibactam sodium belongs to the diazabicyclooctone compound, which itself has no obvious antibacterial activity, but works by inhibiting β-lactamase. Avibactam sodium can inhibit type A (including ESBL and KPC), part of type C and part of type D β-lactamases. Therefore, when used in combination with penicillium, cephalosporin and carbapenem antibiotics, it has broad-spectrum antibacterial activity, especially against Escherichia coli and Klebsiella pneumoniae containing extended-spectrum β-lactamases, containing super The Escherichia coli containing AmpC enzyme and the Escherichia coli containing both AmpC and extended-spectrum β-lactamase have significant activ...

Claims

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Application Information

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IPC IPC(8): C07D471/08
CPCC07D471/08C07B2200/13
Inventor 李发光李海望梁振杨光吴蕾姜珊肖宇陈文博胡佰艳王丽李贺扬吴灵静王晶翼
Owner SICHUAN KELUN PHARMA RES INST CO LTD
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