Cefpirome sulfate preparation technology

A technology of cefpirome sulfate and preparation process, applied in the field of cefpirome sulfate, can solve the problems of unsatisfactory yield, complicated operation and high cost, and achieve the effects of high yield, high purity and good crystal form

Active Publication Date: 2009-02-11
辽宁美亚制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Though, existing patent and document report the refinement process of cefpirome sulfate at present, in these disclosed refinement methods, some need to use silica gel column to separate, have pressurization step, loaded down with trivial details operation, cost is also high, and some are only The refining method in the laboratory cannot be scaled up to actual production, and some methods can be industrialized but the yield is not ideal

Method used

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  • Cefpirome sulfate preparation technology
  • Cefpirome sulfate preparation technology

Examples

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experiment example 1

[0029] Such as figure 1 Shown, a kind of cefpirome sulfate refining technique, carries out according to the following steps:

[0030] 1. Add 20g of cefpirome sulfate coarse powder, 100ml of water and 10ml of methanol into a 250ml three-neck bottle, then add dropwise 3mol / l sodium carbonate solution, stir, and adjust the pH to 3.0-6.0 to dissolve the solid in the bottle.

[0031] 2. Add activated carbon, stir for 30 minutes, and filter. Can continue to add activated carbon to the filtrate as required, stir for 30min, filter, and so many times.

[0032] 3. Use 2mol / l sulfuric acid solution to adjust the pH of the filtrate to 1.0-4.0, add acetone, and crystallize.

[0033] 4. Suction filtration, washing the crystals with acetone, and drying the wet crystals to obtain cefpirome sulfate.

[0034] The molar yield of cefpirome sulfate prepared in this embodiment is 94.3%, the crystal is slightly yellow, and the HPLC detection content is 95.2%, and the solution color is greater tha...

Embodiment 1

[0037] Such as figure 1 Shown, a kind of cefpirome sulfate refining technique, carries out according to the following steps:

[0038] 1. Add 20 g of cefpirome sulfate coarse powder of the same batch as Experimental Example 1, 100 ml of water and 10 ml of methanol in a 250 ml three-necked bottle, then add dropwise 3mol / l sodium carbonate solution, stir, and adjust the pH to 3.0-6.0, Dissolve the solid in the bottle, fill the bottle with nitrogen for protection, then add 0.2 g of sodium metabisulfite, stir, and decolorize.

[0039] 2. Add activated carbon, stir for 30 minutes, and filter.

[0040] 3. Use 2mol / l sulfuric acid solution to adjust the pH of the filtrate to 1.0-4.0, add acetone, and crystallize.

[0041] 4. Suction filtration, washing the crystals with acetone, and drying the wet crystals to obtain cefpirome sulfate.

[0042] The molar yield of cefpirome sulfate prepared in this embodiment is 93.9%, the crystal is white, the HPLC detection content is 97.7%, and th...

Embodiment 2

[0045]In this embodiment, the dosages are 20 g cefpirome sulfate coarse powder, 22 ml ethanol, 0.16 g sodium metabisulfite, and 3 mol / l sodium hydroxide solution.

[0046] Others are the same as embodiment 1.

[0047] The molar yield of cefpirome sulfate prepared in this embodiment is 94.5%, the crystal is white, the HPLC detection content is 94.3%, and the solution color is smaller than the yellow No. 1 standard colorimetric solution.

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Abstract

The invention discloses a preparation technique for cefpirome sulfate, which is carried out according to the following steps: first, a crude product of the cefpirome sulfate is put into water, or proper alcohol and alkaline solution are added to the cefpirome solution and stirred until pH value is between 3.0 and 6.0 so as to cause solid cefpirome sulfate to be dissolved; meanwhile, a discoloring agent is added, and stirring and discoloring are carried out, wherein, the mole ratio of the dosage of the discoloring agent to the dosage of the cefpirome is between 1 to 500 and 1 to 10; second, active carbon is added, stirred for 20min to 60 min and is filtered; third, sulphuric acid solution is used for adjusting the pH value of filter liquid to be 1.0 to 4.0; acetone is added and crystallization is carried out; fourth, vacuum filtration is carried out; acetone is used for cleaning crystals; the wet crystal is dried, thus obtaining the cefpirome sulfate. The preparation technique for preparing the cefpirome sulfate has high yield, high purity and good crystal form and can obtain the cefpirome sulfate without mixed color.

Description

technical field [0001] The invention relates to a preparation process of cefpirome sulfate. Background technique [0002] Cefpirome Sulfate (Cefpirome Sulfate), the molecular formula is C 22 h 22 N 6 o 5 S 2 ·H 2 SO 4 , the chemical name is (6R, 7R)-7-[(Z)-2-(2-aminothiazol-4-yl)-2-methoxyiminoacetamido]-3-(6,7-dihydro- 5H-cyclopentyl[b]pyridinium-1-ylmethyl)-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxymonosulfuric acid Salt, is the sulfate salt of cefpirome. The structural formula is as follows: [0003] [0004] Cefpirome sulfate is the 4th generation broad-spectrum cephalosporin, which was jointly developed by Hearst Company of Germany and Roussel-Euclave Company of France. It was launched in Mexico and Sweden in 1992, and later in many European countries and Japan. , The compound patent of this product is EP64740, which was applied by Hearst Company of Germany, and the priority date was May 10, 1981. Cefpirome sulfate has a broad antibacterial spectr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46
Inventor 郑玉林管海英
Owner 辽宁美亚制药有限公司
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