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Refining process of 7-ACP.HCL

A 7-ACP and process technology, applied in the field of refining 7-ACP HCl, can solve the problems such as no one has published the purification method of 7-ACP HCl, achieve simple operation procedures and reaction conditions, high yield and high purity , the effect of improving the purity

Active Publication Date: 2010-06-30
SHANGHAI NEW ASIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, up to now, no one has published a purification method for 7-ACP·HCl, especially a method capable of industrial production

Method used

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  • Refining process of 7-ACP.HCL

Examples

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Embodiment 1

[0025] In the present embodiment, a refining process of 7-ACP·HCl is carried out according to the following steps:

[0026] 1. Add 200ml of deionized water and 50g of crude 7-ACP·HCl into a 1000ml three-necked flask, then add 15% hydrochloric acid solution dropwise, stir and dissolve, so that the pH of the solution is 1.0.

[0027] 2. Add 15ml of 5% hydrogen peroxide to the solution, stir for 15min, add 5g of activated carbon, stir for 30min, filter, wash the carbon with 50ml of deionized water, and combine the washing solution and the filtrate.

[0028] 3. Add 230ml of dichloromethane to the filtrate, stir for 15min, let stand to separate the layers, and separate the water phase.

[0029] 4. Add 500ml of acetone to the water phase, add dropwise 15% ammonia solution while stirring, adjust the pH value to 3.0, stir and crystallize, and grow the crystal for 2 hours after the crystallization is complete.

[0030] 5. Suction filtration, the filtered crystals were washed with 100m...

Embodiment 2

[0033] In the present embodiment, a refining process of 7-ACP·HCl is carried out according to the following steps:

[0034] 1. Add 180ml of deionized water and 45g of crude 7-ACP·HCl into a 1000ml three-necked bottle, then add 20% hydrochloric acid solution dropwise, stir and dissolve, so that the pH of the solution is 0.5.

[0035] 2. Add 10ml of 10% hydrogen peroxide to the solution, stir for 5 minutes, add 5g of activated carbon, stir for 15 minutes, filter, wash the carbon with 50ml of deionized water, and combine the washing solution and the filtrate.

[0036] 3. Add 200ml of dichloromethane to the filtrate, stir for 30min, let stand to separate the layers, and separate the water phase.

[0037] 4. Add 500ml of acetone to the water phase, add dropwise 5% sodium hydroxide solution while stirring, and adjust the pH value to 4.0. The temperature of the solution was cooled to 10°C in a water bath, and the temperature was maintained throughout the crystallization process, and...

Embodiment 3

[0041] In the present embodiment, a refining process of 7-ACP·HCl is carried out according to the following steps:

[0042] 1. Add 550ml of deionized water and 130g of crude 7-ACP·HCl into a 2500ml three-necked bottle, then add 5% hydrochloric acid solution dropwise, stir and dissolve, so that the pH of the solution is 2.0.

[0043] 2. Add 16ml of 15% hydrogen peroxide to the solution, stir for 5 minutes, add 10g of activated carbon, stir for 15 minutes, filter, wash the carbon with 150ml of deionized water, and combine the washing liquid and the filtrate.

[0044] 3. Add 800ml of dichloromethane to the filtrate, stir for 15min, let stand to separate the layers, and separate the water phase.

[0045] 4. Add 1500ml of acetone to the water phase, add 10% sodium carbonate solution dropwise while stirring, adjust the pH value to 2.5, cool the solution to 5°C in a water bath, keep the temperature during the crystallization process, stir to crystallize, and grow crystals for 2 hours...

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Abstract

The invention discloses a refining process of 7-ACP.HCL, comprising the following steps of: 1, adding a hydrochloric solution to an aqueous 7-ACP.HCL crude product solution, stirring, dissolving, and regulating a pH value between 0.5 and 2.0; 2, adding a right amount of hydrogen peroxide, stirring, then adding activated carbon, stirring for 15-30 minutes, filtering, washing the carbon by using deionized water, and merging washing liquor; 3, adding methylene dichloride, stirring for 15-30 minutes, standing and demixing, and separating an aqueous phase; and 4, adding a right amount of acetone to the aqueous phase, dripping an alkali solution, regulating the pH value between 2.5 and 4.0, stirring, crystallizing, and growing crystals for 1-2 hours after the crystallization. The invention has high yield and purity of the 7-ACP.HCL, is beneficial to synthesizing high-purity cefpirome sulfate, enhances the purity of the 7-ACP.HCL by removing iodide impurities contained in the 7-ACP.HCL by adding the hydrogen peroxide before the recrystallization process of the 7-ACP.HCL, has simple operation process and reaction condition, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for refining 7-ACP·HCl, that is, a method for preparing refined 7-ACP·HCl from crude 7-ACP·HCl. Background technique [0002] Cefpirome sulfate is a fourth-generation broad-spectrum cephalosporin, which has a broad antibacterial spectrum, including Gram-positive cocci and negative cocci, and has antibacterial activity against Enterobacteriaceae that can produce class I β-lactamase ; In addition, including methicillin-sensitive Staphylococcus aureus antibacterial activity is stronger than the third generation cephalosporins. Of all the 3rd and 4th generation cephalosporins, cefpirome sulfate is the most active against Gram-positive bacteria. Moreover, this product has excellent antibacterial activity against Enterobacteriaceae. Most Enterobacteriaceae are highly sensitive to cefpirome sulfate. Bacteria are also very active. In addition, because cefpirome sulfate has good bactericidal activity against bacterial mening...

Claims

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Application Information

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IPC IPC(8): C07D501/46A61P31/04
Inventor 郑玉林管海英陈玉双王立新胡旭华
Owner SHANGHAI NEW ASIA PHARMA
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