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Flucloxacillin sodium compound and preparation thereof

A technology of flucloxacillin sodium and flucloxacillin, which is applied in the field of flucloxacillin sodium compound and its preparation, can solve problems such as reducing product yield, achieve the effects of improving purity, ensuring drug safety, and stabilizing product quality

Inactive Publication Date: 2009-07-08
海南本创医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its common feature is that the drug is purified by forming a salt with bisbenzylethylenediamine, and then undergoes ion exchange to obtain the corresponding salt of the desired drug, but this process reduces the yield of the product

Method used

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  • Flucloxacillin sodium compound and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] i, the preparation of flucloxacillin N'N-dibenzylethylenediamine salt

[0026] Dissolve 951.7 g of 2 mol of flucloxacillin sodium in 15 L of water, adjust the pH value to 3.0 with hydrochloric acid, then add 8.5 L of methanol, and then add 1576.6 g of 4.4 mol N'N-dibenzylethylenediamine diacetate, at 20 Mix and stir the reaction at ~25°C for 3 hours to produce a white solid. Cool the reaction mixture to 10-15°C, filter, wash the white solid three times with water, then wash three times with methanol, and dry it in vacuum at 30-35°C to obtain 1136.8 g of solid. The rate is 98.8%. The melting range of the crystal is 192-198°C. The salt is washed with water and methanol to obtain a product with a melting point of 195-198°C. Analysis shows that the crystal is N'N-dibenzylethylenediamine: flucloxacillin acid is 1;1 mixture.

[0027] ii, the preparation of flucloxacillin sodium salt

[0028] Suspend 1100 g of flucloxacillin N'N-dibenzylethylenediamine salt crystals in 11 L...

Embodiment 2

[0030] i, the preparation of flucloxacillin N'N-dibenzylethylenediamine salt

[0031] Dissolve 1427.4 g of 3 mol of flucloxacillin sodium in 25 L of water, adjust the pH value to 4.0 with acetic acid, then add 9.5 L of acetone, and then add 537.5 g of 1.5 mol of N'N-dibenzylethylenediamine diacetate, at 20 Mix and stir at ~25°C for 5 hours to produce a white solid. Cool the reaction mixture to 10-15°C, filter, wash the white solid three times with water, then wash three times with acetone, and dry under vacuum at 30-35°C to obtain 1536.8 g of solid. The rate is 99.1%. The melting range of the crystal is 192-198°C. The salt is washed with water and then acetone to obtain a product with a melting point of 195-198°C. Analysis shows that the crystal is N'N-dibenzylethylenediamine: flucloxacillin acid is 1.2:1 mixture.

[0032] ii, the preparation of flucloxacillin sodium salt

[0033] Suspend 1200g of flucloxacillin N'N-dibenzylethylenediamine salt crystals in 6L of ethanol, wh...

Embodiment 3

[0035] i, the preparation of flucloxacillin N'N-dibenzylethylenediamine salt

[0036] Dissolve 475.8 g of 1 mol of flucloxacillin sodium in 5 L of water, adjust the pH value to 4.0 to 5.0 with hydrochloric acid, then add 4.5 L of acetonitrile, and then add 4 mol of N'N-dibenzylethylenediamine diacetate 1433 g, at 20 ~ 25 ° C mixed and stirred for 4 hours to produce a white solid, the reaction mixture was cooled to 10 ~ 15 ° C, filtered, the white solid was washed three times with water, then washed three times with acetonitrile, 30 ~ 35 ° C vacuum drying to obtain 566.8 g of solids, product The rate is 98.7%. The melting range of the crystal is 192-198°C. Wash the salt with water and then acetonitrile to obtain a product with a melting point of 195-198°C. Analysis shows that the crystal is N'N-dibenzylethylenediamine: flucloxacillin acid is 1:1.1 mixture.

[0037] ii, the preparation of flucloxacillin sodium salt

[0038] Suspend 500 g of flucloxacillin N'N-dibenzylethylene...

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Abstract

The invention discloses a flucloxacillin sodium compound and a method for preparing the same. The method comprises that: firstly, N'N-dibenzylethylene diamine salt and flucloxacillin acid are mixed and reacted to form a salt; and secondly, high-purity flucloxacillin sodium is obtained through the displacement of a cation exchange resin. The invention adopts a purification method which is simple and easy to operate, thereby greatly improving the purity of the flucloxacillin sodium compound to a certain degree, removing a large amount of high molecular polymers, stabilizing the product quality of related preparations and ensuring the safety of clinic medication use.

Description

technical field [0001] The invention relates to a flucloxacillin sodium compound and a preparation method thereof. Background technique [0002] Flucloxacillin sodium, chemical name: (2S, 5R, 6R)-6-[[3-(2-chloro-6-fluorophenyl)-5-methyl-1,2-oxazole-4-methanol Acyl]amino]-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid sodium salt, belonging to the fourth generation of isoxazole penicillins , It has a strong bactericidal effect by inhibiting the biosynthesis of bacterial cell wall mucin. The structural formula of flucloxacillin sodium is: [0003] [0004] Flucloxacillin sodium has been included in the 2000 edition of the British Pharmacopoeia. At present, there are injections and oral preparations on the market. There are few domestic manufacturers, and most of them have the defect of poor purity resulting in unstable quality. A large number of polymers have seriously affected its clinical application. Safety. The high polymer is separated, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/76C07D499/16C07D499/20A61P31/04
Inventor 王明
Owner 海南本创医药科技有限公司
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