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Method for preparing crystal form A or crystal form D type avibactam product through crystallization

A technology for avibactam sodium and avibactam sodium salt is applied in the field of preparing crystal form A or crystal form D avibactam products, and achieves the effects of broad market prospect, wide application range and high yield

Inactive Publication Date: 2018-04-20
上海龙翔生物医药开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the development of new antimicrobial agents is a challenging task

Method used

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  • Method for preparing crystal form A or crystal form D type avibactam product through crystallization
  • Method for preparing crystal form A or crystal form D type avibactam product through crystallization
  • Method for preparing crystal form A or crystal form D type avibactam product through crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Use water (1 mL) and avibactam sodium salt (1 g) to prepare avibactam sodium salt solution, take absolute ethanol (9 mL), add avibactam sodium salt solution dropwise to absolute ethanol within 20 min, After the dropwise addition, stir at room temperature for 2 hours, then lower the temperature to 0-5°C and stir for 2 hours, filter, and wash the obtained filter cake with ethanol (5mL×2, that is, wash twice, each time with 5mL ethanol for washing), After washing, vacuum-dry at 45°C for 16 hours to obtain 0.83 g of white solid, with a yield of 83%. According to XRD analysis, it is the monohydrate "A" crystal form avibactam product, the XRD picture is as follows figure 1 shown.

Embodiment 2

[0035] Use water (2 mL) and avibactam sodium salt (1 g) to prepare avibactam sodium salt solution, take absolute ethanol (8 mL), add avibactam sodium salt solution dropwise to absolute ethanol within 20 min, After the dropwise addition, stir at room temperature for 2 hours, then lower the temperature to 0-5°C and stir for 2 hours, filter, and wash the obtained filter cake with ethanol (5mL×2, that is, wash twice, each time with 5mL ethanol for washing), After washing, it was dried under vacuum at 45°C for 16 hours to obtain 0.18 g of white solid with a yield of 18%. According to XRD analysis, it is the monohydrate "A" crystal form avibactam product, the XRD picture is as follows figure 2 shown.

Embodiment 3

[0037] Use water (1mL) and avibactam sodium salt (1g) to prepare the avibactam sodium salt solution, take acetone (19mL), add the avibactam sodium salt solution to the acetone dropwise within 20min, after the dropwise addition , stirred at room temperature for 2h, then cooled to 0-5°C and stirred for 2h, filtered, and the obtained filter cake was washed with acetone (5mL×2, that is, washed twice, each time with 5mL acetone for washing), after washing, in Vacuum drying at 45°C for 16 hours gave 0.71 g of a white solid with a yield of 71%. According to XRD analysis, it is the monohydrate "A" crystal form avibactam product, the XRD picture is as follows image 3 shown.

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Abstract

The invention discloses a method for preparing a crystal form A or crystal form D avibactam product through crystallization. The method comprises the following steps: preparing an avibactam sodium salt solution by adopting a first solvent; weighing a second solvent; mixing the avibactam sodium salt solution and the second solvent by adopting a dropwise adding manner; after dropwise adding, stirring at room temperature; then cooling to 0 to 5 DEG C and continually stirring; filtering to obtain a filter cake; washing the filter cake by adopting the second solvent; after washing, drying in vacuumto obtain a white solid, namely the product. According to the method disclosed by the invention, the avibactam product is prepared through a crystallization manner; the yield is high, the operation method is simple and large-scale industrial production is easy to realize; the solvents used in a preparation process are adjusted, so that the crystal form A and crystal form D avibactam products canbe obtained respectively; when the large-scale industrial production is carried out, the avibactam products with different crystal forms can be obtained respectively only if simple solvent adjustmentis carried out; the method has a wide application range and a wide market prospect.

Description

technical field [0001] The invention relates to the technical field of avibactam production, in particular to a method for preparing crystal form A or crystal form D avibactam products through crystallization. Background technique [0002] Penicillins or cephalosporins are the most frequently used β-lactam antibiotics in clinical practice, but various bacteria have developed resistance to β-lactam antibiotics, and the emergence of bacterial resistance to known antibacterial agents is becoming an important strategy for the treatment of bacterial infections. main challenge. One approach facing the treatment of bacterial infections, especially those caused by drug-resistant bacteria, is the development of newer antimicrobial agents capable of overcoming bacterial resistance. However, the development of new antimicrobial agents is a challenging task. [0003] Avibactam (AVibactam, NXL-104) belongs to the diazabicyclooctone compound and is currently the most promising new type ...

Claims

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Application Information

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IPC IPC(8): C07D471/08
Inventor 熊毅纪兴跃
Owner 上海龙翔生物医药开发有限公司
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