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Preparation method for 6-amino penicillanic acid

A technology for the fermentation of aminopenicillanic acid and penicillin, which is applied in the field of preparation of 6-aminopenicillanic acid, can solve the problems of adding degreasing steps, cumbersome production process, complicated refining steps, etc., and achieves reduced production costs and significant social benefits , the effect of reducing environmental pollution and potential safety hazards

Active Publication Date: 2013-02-13
NORTH CHINA PHARMA COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method still has the following deficiencies: one, still continue to use penicillin fermented liquid through the refining process of traditional filtration, extraction, back extraction, not only refining steps are numerous and diverse, and the yield loss of refining has limited the yield of 6-APA to improve ,Reduce costs
2. In order to adapt to the conditions of invertase, the degreasing step is inevitably added, and thus the deesterified penicillin saline solution can be prepared for enzymatic conversion, and the production process is still relatively cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Cool the penicillin fermentation broth to 5-10°C, go through 8000 molecular weight membrane ultrafiltration to remove most of the soluble macromolecular proteins, and then concentrate through nanofiltration membrane to obtain a concentrated filtrate with a titer of 100,000 u / ml. Put 3000L of concentrated filtrate in a reaction tank, add 10.5MU of immobilized penicillin acylase, and carry out the transformation reaction. After 60 minutes, the 6-APA conversion solution was obtained after filtering to remove impurities. Cool down the 6-APA conversion solution to 5-10°C, add 8 kg of activated carbon and stir for 30 minutes to remove some colored impurities, obtain about 2950L of 6-APA filtrate after filtration, and control the temperature of 6-APA filtrate to 5±2°C , use hydrochloric acid to adjust the pH to 5.8-6.0, add seed crystals, grow crystals for 30 minutes, continue to use hydrochloric acid to adjust the pH to 4.7, add crystallization agent acetone 1500L, continue t...

Embodiment 2

[0020] Cool the penicillin fermentation broth to 10°C, pass through a 10,000 molecular weight membrane ultrafiltration to remove most of the soluble macromolecular proteins, and then concentrate through a nanofiltration membrane to obtain a concentrated solution with a titer of 130,000 u / ml. Put 3050L of concentrated filtrate in a reaction tank, add 13.725MU of immobilized penicillin acylase, and carry out the transformation reaction. After 60 minutes, the 6-APA conversion solution was obtained after filtering to remove impurities. Cool the conversion liquid to 5-10°C, add 10 kg of activated carbon and stir for 30 minutes to remove some colored impurities, and obtain about 3000 L of 6-APA filtrate after filtration. Control the temperature of the 6-APA filtrate to 5±2°C, adjust the pH to 5.8-6.0 with hydrochloric acid, add seed crystals, grow crystals for 30 minutes, continue to adjust the pH to 4.7 with hydrochloric acid, add crystallization agent methanol 3000L, and continue ...

Embodiment 3

[0022] Cool the penicillin fermentation broth to 5°C, pass through a 20,000 molecular weight membrane ultrafiltration to remove most of the soluble macromolecular proteins, and then concentrate through a nanofiltration membrane to obtain a concentrated solution with a titer of 130,000 u / ml. Put 3050L concentrated filtrate in the reaction tank, add 12.16MU of immobilized penicillin acylase, and carry out the transformation reaction. 60. After removing impurities by filtration, the 6-APA conversion solution was obtained. Cool the conversion liquid to 5-10°C, add 11 kg of activated carbon and stir for 30 minutes to remove some colored impurities, and obtain about 3000 L of 6-APA filtrate after filtration. Control the temperature of the 6-APA filtrate to 5±2°C, adjust the pH to 5.8-6.0 with hydrochloric acid, add seed crystals, grow crystals for 30 minutes, continue to adjust the pH to 4.7 with hydrochloric acid, add 2000L crystallization agent ethanol, and continue to adjust the ...

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Abstract

The invention discloses a preparation method for 6-amino penicillanic acid, which comprises the following steps: a, performing ultrafiltration membrane separation and nanofiltration membrane concentration on a penicillin fermentation liquor to obtain a concentrated filter liquor; b, placing the concentrated filter liquor into a reaction tank, adding an immobilized penicillin acylase 4MU / m<3> concentrated filter liquor and performing conversion reaction to obtain a 6-amino penicillanic acid conversion solution; c, performing actived carbon decoloration and filtering on the conversion solution to obtain a 6-amino penicillanic acid filter liquor; and d, adding seed grain into the 6-amino penicillanic acid filter liquor obtained through the procedures in the step c, growing the grain, crystallizing, filtering, washing and drying. The preparation method has the advantages of simple process flow, easiness for operation, safety, environmental protection, and capabilities of effectively improving the yield of 6-APA, reducing the production cost and improving the labor productivity.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical raw materials, in particular to a preparation method of 6-aminopenicillanic acid. Background technique [0002] 6-aminopenicillanic acid, commonly known as penicillin without side chain, or 6-APA for short, is the mother nucleus of penicillin and an important intermediate for the production of various semi-synthetic penicillins. 6-APA itself has very low antibacterial activity and cannot be directly used clinically. However, by using it as a raw material for chemical structure modification and connecting side chains of different structures, a series of products with strong antibacterial activity and new disease resistance can be produced. Take convenient semi-synthetic penicillins such as benzyl penicillin, methicillin, amoxicillin, mezlocillin, ampicillin, etc., thus creating a new era of semi-synthetic antibiotics. [0003] As an important intermediate for the preparation of semi-synthe...

Claims

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Application Information

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IPC IPC(8): C12P37/06
Inventor 闫峰段志钢萧泛舟谷中芝赵伟郭文仿尹科科杨立婷刘海莲陈浩
Owner NORTH CHINA PHARMA COMPANY
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