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Refining method of biapenem crude product

A technology of biapenem and refining method, applied in the field of chemical pharmacy, can solve problems such as troublesome operation, and achieve the effects of small crystal size, high yield and reducing solvent residues

Active Publication Date: 2022-04-15
ZHUHAI UNITED LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to use sodium hydroxide solution to adjust the pH value, and the operation is relatively troublesome.

Method used

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  • Refining method of biapenem crude product
  • Refining method of biapenem crude product
  • Refining method of biapenem crude product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A method for refining crude biapenem, comprising the steps of:

[0045] 1. Put 3 g of crude biapenem into 100 mL of water for injection (controlled temperature at 25°C), and stir until dissolved to obtain a mixture.

[0046] 2. Add 0.03 g of activated carbon to the mixture, stir and dissolve, then filter to obtain feed liquid; keep the feed liquid temperature at 25°C.

[0047] 3. The feed solution was dropped into 100 mL of ethanol (at a controlled temperature of 5° C.) to obtain a reaction system.

[0048] 4. Raise the temperature of the reaction system to 20°C and keep it; put 7g of crude biapenem into 300mL of water for injection (control temperature 25°C), stir until it dissolves to obtain a mixture; add 0.27g of activated carbon to the mixture, stir to dissolve and filter , to obtain the feed liquid; dropwise add the feed liquid obtained in this step to the reaction system.

[0049] 5. Keep the temperature of the reaction system at 20°C, grow the crystal for 30 m...

Embodiment 2

[0052] A method for refining crude biapenem, comprising the steps of:

[0053] 1. Put 2 g of crude biapenem into 120 mL of water for injection (controlled temperature at 20°C), and stir until dissolved to obtain a mixture.

[0054] 2. Add 0.05 g of activated carbon to the mixture, stir to dissolve and then filter to obtain the feed liquid; keep the feed liquid temperature at 20°C.

[0055] 3. Drop the feed solution into 960 mL of ethanol (control temperature -4°C) to obtain a reaction system.

[0056] 4. Raise the temperature of the reaction system to 25°C and maintain it; put 8g of crude biapenem into 480mL of water for injection (control temperature 20°C), stir until it dissolves to obtain a mixture; add 0.45g of activated carbon to the mixture, stir to dissolve and then filter , to obtain the feed liquid; dropwise add the feed liquid obtained in this step to the reaction system.

[0057] 5. Keep the temperature of the reaction system at 25°C, grow the crystal for 30 minutes...

Embodiment 3

[0059] A method for refining crude biapenem, comprising the steps of:

[0060] 1. Put 1 g of crude biapenem into 45 mL of water for injection (at a controlled temperature of 30°C), and stir until dissolved to obtain a mixture.

[0061] 2. Add 0.02 g of activated carbon to the mixture, stir, dissolve and filter to obtain a feed liquid; keep the temperature of the feed liquid at 30°C.

[0062] 3. Drop the feed solution into 1350mL ethanol (control temperature -7°C) to obtain a reaction system.

[0063] 4. Raise the temperature of the reaction system to 15°C and keep it; put 9g of crude biapenem into 405mL of water for injection (control temperature 30°C), stir until the mixture is dissolved; add 0.18g of activated carbon to the mixture, stir to dissolve and then filter , to obtain the feed liquid; dropwise add the feed liquid obtained in this step to the reaction system.

[0064] 5. Keep the temperature of the reaction system at 15°C, grow the crystal for 30 minutes after the ...

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Abstract

The invention belongs to the technical field of chemical pharmacy, and particularly relates to a refining method of a biapenem crude product. According to the invention, a biapenem refining process is optimized, and crystallization is carried out by stages under different temperature conditions by adopting a reverse crystallization mode of dropwise adding a feed liquid into a crystallization agent. The temperature of first crystallization is-10 to 10 DEG C, crystallization is carried out at a low temperature, crystals can be rapidly separated out, the form of the crystals is easy to control, and the granularity of the crystals of the obtained product is small; the temperature of secondary crystallization is 5-30 DEG C, and crystallization is carried out at a relatively high temperature, so that solvent residues of the product can be reduced. The product prepared by the method disclosed by the invention is short in redissolution time, high in purity, high in yield and good in stability, the crystal form of the product is consistent with that of an original product, and a powerful guarantee is provided for product consistency evaluation.

Description

technical field [0001] The invention relates to the technical field of chemical industry and pharmacy, in particular to a method for refining crude biapenem. Background technique [0002] Biapenem, English name: biapenem, chemical name: (-)-6-[(4R,5S,6S)-2-mercapto-6-[(R)-1-hydroxyethyl]-4-methyl -7-Oxo-1-azabicyclo[3.2.0]hept-2-en-3-yl]-thio-[6,7-dihydro-5H-pyrazol[1,2-a]] [1,2,4] triazole inner salt. Biapenem is a 1β-methyl carbapenem antibiotic, developed by Japan Lederle Company and American Cyamide Company, and was launched in Japan jointly by Japan Lederle Company and Japan Meiji Co., Ltd. in March 2002. It is widely used clinically in acute and chronic infections caused by Gram-negative aerobic bacteria and Gram-positive aerobic bacteria, and its activity against Gram-negative bacteria is better than that of imipenem, and its activity against Gram-positive bacteria Similar to imipenem, it has good curative effect on plastic surgery infection, gynecological infectio...

Claims

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Application Information

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IPC IPC(8): C07D519/06
Inventor 何晨黄颜炯刘翔粟立山韩玉波
Owner ZHUHAI UNITED LAB
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