Technique for preparing high-purity cefpirome sulfate

A technology of cefpirome sulfate and organic solvents, which is applied in the field of refining cefpirome sulfate, can solve the problems of high energy consumption, etc., and achieve the effects of short production time, large output, and good industrial application value

Inactive Publication Date: 2008-01-16
SHENZHEN SALUBRIS PHARMA CO LTD +1
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This method consumes a lot of energy

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  • Technique for preparing high-purity cefpirome sulfate

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Embodiment 1

[0021] Add 300g of crude cefpirome sulfate (0.49mol, the weight is based on anhydrous matter) to 1500mL of water at room temperature (15-25°C), and add about 20% sodium hydroxide aqueous solution dropwise under vigorous stirring until the pH of the system is 6.5-7.0 between. Then add 3000mL acetone and appropriate amount of activated carbon, and stir for 30 minutes. The solid was isolated by centrifugation or suction filtration. Wash the filter cake with 800 mL of acetone-water 2:1 (v / v) mixed solution, and combine the filtrates. Add 30% H to the filtrate with stirring 2 SO 4 to pH 1.0-1.5. Then 9 L of acetone was added. After the crystals were precipitated, the temperature of the system was lowered to 5-10°C, and the stirring was continued for 1 hour. Suction. The filter cake was washed with acetone and dried under vacuum at 40° C. to obtain about 270 g of white crystalline powder. The purity is above 99%, and the water content is 3-4%. The product is cefpirome sulfa...

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Abstract

The present invention relates to a method for refining cefpirome sulfate. Sodium hydroxide and cefpirome sulfate are reacted to generate sodium sulfate and free cefpirome, and then organic solvent is added so that the generated sodium sulfate and the hydrate are precipitated. Cefpirome sulfate can be gained when the sulfuric acid salt formation is re-added to the decolored filtrate.

Description

technical field [0001] The invention relates to a preparation method of cephalosporin compounds, especially a method for refining cefpirome sulfate. Background technique [0002] Cefpirome (cefpirome, formula I) is the fourth-generation cephalosporin antibiotic for injection, developed by the Federal Republic of Germany Hoechst Company (DE 3118732), and is known to be antibacterial to Gram-positive bacteria among the third and fourth-generation cephalosporins. Most active antibiotic. Cefpirome is a water-soluble internal salt with quaternary ammonium cation and carboxyl anion, and its sulfate salt is used clinically as an intravenous injection. [0003] [0004] Cefpirome is not a naturally occurring substance in nature and is usually prepared by semi-synthetic methods. In Example 50 of US Patent No. 5,071,979, cefpirome is obtained through quaternization reaction, and free cefpirome is separated by silica gel chromatography. In Example 8 of US Pat. No. 4,609,653, free...

Claims

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Application Information

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IPC IPC(8): C07D501/46
Inventor 谭端明李刚叶澄海
Owner SHENZHEN SALUBRIS PHARMA CO LTD
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