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Method for preparing high-purity cefpirome sulfate by sodium salt precipitation method

A technology of cefpirome sulfate and precipitation method, applied in organic chemistry, antibacterial drugs, etc., can solve the problems of high energy consumption and achieve the effects of large equipment output, good industrial application value, and short production time

Inactive Publication Date: 2009-04-01
SHENZHEN SALUBRIS PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method consumes a lot of energy

Method used

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  • Method for preparing high-purity cefpirome sulfate by sodium salt precipitation method

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Embodiment 1

[0029] Add 300g of cefpirome sulfate crude product (0.49mol, the weight is based on anhydrous matter) to 1500mL of water at room temperature (15-25°C), add about 20% sodium hydroxide aqueous solution dropwise under vigorous stirring until the pH of the system is 6.5- Between 7.0 (the amount of sodium hydroxide is about 39g, 0.98mol). Then add 3000mL acetone and an 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 pH1.0-1.5. 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%, ...

Embodiment 2

[0031] At room temperature (15-25°C), add 300g of cefpirome sulfate crude product (0.49mol, weight based on anhydrous matter) into 1500mL of water, and then add 150ml of acetone. Add NaHCO in batches with stirring 3 82.3 g (0.98 mol). Stir for 20 minutes. Then add 2850mL 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 600 mL of acetone-water 2:1 (v / v) mixed solution, and combine the filtrates. Add 50% H to the filtrate with stirring 2 SO 4 to pH1.0-1.5. 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. Result is with embodiment 1.

Embodiment 3

[0033] Add 300g of cefpirome sulfate crude product (0.49mol, weight based on anhydrous matter) to 1500mL of water at room temperature (15-25°C), and then add 100ml of acetone. Add Na in batches under stirring 2 CO 3 48 g (0.45 mol). Stir for 20 minutes. Then add 3000mL acetone and an appropriate amount of activated carbon, and stir for 30 minutes. The solid was isolated by centrifugation or suction filtration. Wash the filter cake with 600 mL of acetone-water 2:1 (v / v) mixed solution, and combine the filtrates. Add 40% H to the filtrate with stirring 2 SO 4 to pH1.0-1.5. 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. Result is with embodiment 1.

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Abstract

The invention relates to a method adopting a sodium-salt precipitation method to prepare high-pure cefpirome sulfate. The method uses sodium-salt to react with the cefpirome sulfate to generate the sodium sulfate and free cefpirome, and then an organic solvent is added to generate the sodium sulfate and hydrates thereof by precipitation. The sulfate is added again in a decolored filtrate to obtain the cefpirome sulfate.

Description

technical field [0001] The invention relates to a preparation method of cephalosporin compounds, in particular to a method for preparing high-purity cefpirome sulfate by a sodium salt precipitation method. 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 chr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46A61P31/04
Inventor 谭端明李刚叶澄海
Owner SHENZHEN SALUBRIS PHARMA CO LTD
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