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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 high energy consumption, long freeze-drying cycle, environmental hazards, etc., achieve low production cost, simple steps, The effect of reducing acid-alkaline wastewater

Active Publication Date: 2018-08-17
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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  • Method for preparing amorphous avibactam sodium by spray-drying
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  • Method for preparing amorphous avibactam sodium by spray-drying

Examples

Experimental program
Comparison scheme
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) is 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 solid drying The dry weight is 10.51g, and the yield is 93%. The solid substance: amorphous, disorderly arrangement.

Embodiment 3

[0054] The ethyl acetate (200ml) solution of sodium isooctanoate (7.6g, 44mmol) was added dropwise in the ethyl acetate 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 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 infections (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. ...

Claims

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Application Information

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Patent Type & Authority Applications(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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