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Preparation process of azlocillin sodium

A technology of azlocillin sodium and preparation process, applied in the direction of organic chemistry and the like, can solve the problems of poor storage stability, high impurity content, poor use safety, etc., and achieve the effects of improving stability, increasing yield and reducing production cost

Inactive Publication Date: 2020-07-03
SUZHOU ERYE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The storage stability of azlocillin sodium in the prior art is poor, and its related substances will increase significantly in the light and humid environment, and the long-term storage impurity content is high, and the use safety is poor

Method used

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  • Preparation process of azlocillin sodium
  • Preparation process of azlocillin sodium
  • Preparation process of azlocillin sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Add 500L of purified water and 100L of acetone into the glass-lined reactor, stir and cool down to 0-5°C;

[0049] (2) Add 50kg of ampicillin trihydrate, add about 13kg of triethylamine at 0-5°C, stir and dissolve for 30min, and the pH is 8.0-9.0;

[0050](3) After the reaction solution was dissolved, quickly add 19 kg of 1-chloroformyl-2-imidazolidinone into the reaction kettle. After the addition is complete, stir at 0-5°C for 1 hour, add about 13 kg of triethylamine, continue to stir and dissolve for 30 minutes, and the pH is 8.0-9.0;

[0051] (4) After dissolving, filter the reaction solution into the crystallization tank through a 0.45 μm filter element;

[0052] (5) Add 1000L of 95% ethanol to the crystallization tank, stir and cool down to 10-15°C;

[0053] (6) Slowly add 1N hydrochloric acid dropwise at 10-15°C, adjust pH=2.5-3.0, and continue stirring for 0.5 hours;

[0054] (7) Put the material into a centrifuge for centrifugation. After the centrifuga...

Embodiment 2

[0068] (1) Add 500L of purified water and 100L of acetone into the glass-lined reactor, stir and cool down to 0-5°C;

[0069] (2) Add 50kg of ampicillin trihydrate, add about 13kg of triethylamine at 0-5°C, stir and dissolve for 30min, and the pH is 8.0-9.0;

[0070] (3) After the reaction solution was dissolved, quickly add 19 kg of 1-chloroformyl-2-imidazolidinone into the reaction kettle. After the addition is complete, stir at 0-5°C for 1 hour, add about 13 kg of triethylamine, continue to stir and dissolve for 30 minutes, and the pH is 8.0-9.0;

[0071] (4) After dissolving, filter the reaction solution into the crystallization tank through a 0.45 μm filter element;

[0072] (5) Add 1000L of 95% ethanol to the crystallization tank, stir and cool down to 10-15°C;

[0073] (6) Slowly add 1N hydrochloric acid dropwise at 10-15°C, adjust pH=2.5-3.0, and continue stirring for 0.5 hours;

[0074] (7) The material is released to the centrifuge for centrifugation. After the c...

Embodiment 3

[0088] (1) Add 500L of purified water and 100L of acetone into the glass-lined reactor, stir and cool down to 0-5°C;

[0089] (2) Add 50kg of ampicillin trihydrate, add about 13kg of triethylamine at 0-5°C, stir and dissolve for 30min, and the pH is 8.0-9.0;

[0090] (3) After the reaction solution was dissolved, quickly add 19 kg of 1-chloroformyl-2-imidazolidinone into the reaction kettle. After the addition is complete, stir at 0-5°C for 1 hour, add about 13 kg of triethylamine, continue to stir and dissolve for 30 minutes, and the pH is 8.0-9.0;

[0091] (4) After dissolving, filter the reaction solution into the crystallization tank through a 0.45 μm filter element;

[0092] (5) Add 1000L of 95% ethanol to the crystallization tank, stir and cool down to 10-15°C;

[0093] (6) Slowly add 1N hydrochloric acid dropwise at 10-15°C, adjust pH=2.5-3.0, and continue stirring for 0.5 hours;

[0094] (7) The material is released to the centrifuge for centrifugation. After the c...

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Abstract

The invention provides a preparation method of azlocillin sodium. The preparation method mainly comprises two steps including synthesis of azlocillin acid and salification of azlocillin. A preparationmethod for azlocillin acid comprises the following steps: adding ampicillin trihydrate acid and acetone into purified water; adding triethylamine to dissolve ampicillin trihydrate acid; adding 1-chloroformyl-2-imidazolidinone, and carrying out a reaction; adding triethylamine for dissolving and clarifying; adding a crystallization solvent, namely ethanol or isopropanol; and adjusting acidity, carrying out crystallizing, and performing centrifugal drying to obtain azlocillin acid. The preparation method for azlocillin sodium comprises the following steps: adding azlocillin acid into water forinjection; adding sodium bicarbonate and an aqueous sodium hydroxide solution for salifying; carrying out sterilizing, filtering and freeze-drying; and taking a product out of a box to obtain azlocillin sodium. According to the preparation method provided by the invention, higher yield and quality are guaranteed, and remarkable effects can be achieved, especially in the aspect of the control of sensitization impurities (polymers), pH values and solubility. Therefore, the prepared azlocillin sodium product is high in stability and safer to use.

Description

technical field [0001] The present disclosure relates to the technical field of medicine, in particular to a preparation process of azlocillin sodium compound. Background technique [0002] Azlocillin sodium, English name: Azlocillin Sodium, molecular formula: C 20 h 22 N 5 NaO 6 S, chemical name: (2S,5R,6R)-3,3-dimethyl-6-{(R)-2-(2-oxo-1-imidazolecarboxamido)-2-phenylacetamido} -7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid sodium salt, the structural formula is as shown in the following I: [0003] [0004] Azlocillin sodium is a broad-spectrum, high-efficiency semi-synthetic penicillin, mainly used for various infections caused by sensitive Gram-negative bacteria and positive bacteria, as well as Pseudomonas aeruginosa infection, including sepsis, meningitis, cardiac Meningitis, suppurative pleurisy, peritonitis, lower respiratory tract, gastrointestinal tract, biliary tract, kidney and urethra, bone and soft tissue and reproductive organs and other in...

Claims

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Application Information

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IPC IPC(8): C07D499/16C07D499/18C07D499/68
CPCC07D499/16C07D499/18C07D499/68
Inventor 马磊范胜亚朱晓晨乔德强
Owner SUZHOU ERYE PHARMA CO LTD
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