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A method for preparing amorphous avibactam sodium by spray drying

A kind of avibactam sodium, amorphous technology, applied in the field of preparation of amorphous avibactam sodium, can solve the problems of environmental hazards, long freeze-drying cycle, high energy consumption, etc., achieve low production cost, simple steps, Ease of industrial production

Active Publication Date: 2019-11-08
山东安信制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In the above-mentioned patent documents, the preparation method of amorphous avibactam sodium is: after using sodium ion exchange, it is prepared by freeze-drying. The preparation process will produce a large amount of acidic wastewater and alkaline wastewater, which is harmful to the environment. Freeze-drying in a dryer, the freeze-drying cycle is about 48 hours longer, and the energy consumption is large

Method used

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  • A method for preparing amorphous avibactam sodium by spray drying
  • A method for preparing amorphous avibactam sodium by spray drying
  • A method for preparing amorphous avibactam sodium by spray drying

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A dichloromethane (100ml) solution of sodium isooctanoate (3.8g, 22mmol) was added dropwise to avibactam tetrabutylammonium salt (10g, 19.7mmol) in a dichloromethane solution (100ml), keeping the reaction temperature at At 20°C, the dropwise addition was completed in 20 minutes. After dripping and keeping warm for 3 hours, add 200ml of purified water for extraction, and the water phase enters the spray dryer (control the air inlet temperature at 150°C, the air outlet temperature at 80°C, and the injection volume at 75ml / min) to obtain 5.2g of solid matter. Yield 92%. The solid substance: amorphous, disorderly arrangement.

[0036] The above-mentioned solid is detected by two methods of XRD spectrum and DSC spectrum, as follows:

[0037] 1. The detection method of XRD pattern is as follows:

[0038] Instrument: PANalytical powder X-ray diffractometer;

[0039] Model: XpertPROMPD;

[0040] Test method: the target material is copper, the light pipe is set (40kv, 40mA)...

Embodiment 2

[0052] The n-butanol (200ml) solution of sodium isooctanoate (7.6g, 44mmol) was added dropwise in the n-butanol solution (200ml) of avibactam tetrabutylammonium salt (20g, 39.4mmol), keeping the reaction temperature at 20°C, 20min dropwise addition, heat preservation reaction for 3h, add 400ml of purified water for extraction, the water phase enters the spray dryer (air inlet temperature is 150°C, air outlet temperature is 80°C, injection volume is 75ml / min) to obtain a solid drying The dry weight is 10.51g, and the yield is 93%. The solid substance: amorphous, disorderly arrangement.

Embodiment 3

[0054] A solution of ethyl acetate (200ml) of sodium isooctanoate (7.6g, 44mmol) was added dropwise to a solution of ethyl acetate (200ml) of avibactam tetrabutylammonium salt (20g, 39.4mmol), keeping the reaction temperature at 20°C, 20min dropwise addition, heat preservation reaction for 3h, add 400ml of purified water for extraction, the water phase enters the spray dryer (air inlet temperature is 150°C, air outlet temperature is 80°C, injection volume is 75ml / min) to obtain a solid drying The dry weight is 10.29g, and the yield is 91%. The solid substance: amorphous, disorderly arrangement.

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Abstract

The invention discloses a method for preparing amorphous avibactam sodium by spray-drying. According to the invention, solution of sodium iso-octoate is dropwise added into solution of avibactam tetrabutylammonium salt, after dropwise adding is completed, the reaction is performed for 3 to 4h, and purified water is added for extraction; after a water phase is subjected to spray-drying, the amorphous avibactam sodium is obtained. The method disclosed by the invention is simple in step and easy for industrial production, the purity of a product is greater than or equal to 98.0%, and yield is greater than or equal to 90.0%.

Description

technical field [0001] The invention relates to a preparation method of amorphous avibactam sodium, which belongs to the technical field of medicinal chemistry. Background technique [0002] Avibactam sodium, English name is avibactam sodium, chemical name: [(1R,2S,5R)-2-(aminocarbonyl)-7-oxo-1,6-diazabicyclo[3.2.1]octane -6-base] sulfuric acid monosodium salt, the chemical structural formula is [0003] [0004] Avibactam sodium and ceftazidime, a cephalosporin antibacterial drug, form a compound preparation with a fixed ratio, which was approved by the US FDA on February 15, 2015, for the treatment of complicated intra-abdominal infections and complicated urinary tract infections in adults , for the treatment of patients with kidney infection (pyelonephritis). [0005] Avibactam (avibactam, NXL-104) belongs to the diazabicyclooctone compound, which itself has no obvious antibacterial activity, but can inhibit type A (including ESBL and KPC) and type C β-lactamases. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/08
CPCC07D471/08
Inventor 周显峰李法东刘瑜张重坤潘广朋李卓华杨庆坤吴柯李保勇
Owner 山东安信制药有限公司
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