6-aminopenicillanic acid preparation method

A technology of aminopenicillanic acid and penicillin, which is applied in the direction of organic chemistry, can solve the problems of solvent power and energy waste, increase production cost, and yield loss, etc., so as to reduce the number of crystallization times, avoid yield loss, and reduce The effect of production costs

Inactive Publication Date: 2006-02-15
NORTH CHINA PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This leads to a lot of yield loss and low product yield in the double crystallization...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Penicillium fermentation broth is filtered, acidified, and butyl ester is concentrated and extracted to obtain a titer of 70,000 to 100,000 units of butyl penicillinate extract (i.e. one BA), add activated carbon at 40-100g / billion units, and add activated carbon at -20- Stir at 10°C for 20-60 minutes, filter; to remove part of the colored impurities in primary BA, filter, add 9-12% potassium carbonate solution to the filtrate at 1.0-1.5 liters / billion units, stir, stand still and separate phases, Back extraction gets penicillin potassium aqueous solution (RB), makes RB potency control at 45--550,000 units, guarantees deesterification effect; RB flows through ADS-18 (produced by Tianjin Nankai Synthetic Technology Co., Ltd.) with the speed of 200-400L / h sold) for degreasing to remove the residual butyl ester in RB, wash the resin column with purified water, and the volume of penicillin potassium aqueous solution (i.e. eluent) after degreasing reaches 1.5-3 times of the v...

Embodiment 2

[0022] Penicillium fermentation broth was filtered, acidified, and butyl ester was concentrated and extracted to obtain a penicillin butyl ester extract with a titer of 73,000 units, that is, a BA. Add activated carbon at 40g / billion units, stir at -20-10°C for 20 minutes, and filter To remove part of the colored impurities in the primary BA, filter, add 9% sodium carbonate solution in the filtrate by 1.0 liters / billion units, stir, leave standstill for phase separation, and separate penicillin sodium aqueous solution (RB), the RB titer is 550,000 units; RB flows through the AXT-33 (commercially available) resin column at a speed of 400L / h for degreasing to remove the residual butyl ester in RB, and washes the resin column with purified water to make the volume of the eluent reach 3 times the volume before loading the column; put the eluate in a reaction tank equipped with penicillin acylase, add boric acid buffer according to 3% of the total volume of the eluate after degreasi...

Embodiment 3

[0024] Penicillium fermentation broth is filtered, acidified, and butyl ester is concentrated and extracted to obtain a butyl penicillinate extract with a titer of 100,000 units, that is, a BA. Add activated carbon at 100g / billion units, and stir at -20-10°C for 50 minutes. Filtration; to remove part of the colored impurities in the primary BA, filter, add 12% sodium carbonate solution to the filtrate by 1.5 liters / billion units, stir, leave to stand for phase separation, and separate to obtain penicillin sodium aqueous solution (RB), RB titer It is 500,000 units; RB flows through the AXT-33 resin column at a rate of 200L / h for degreasing to remove the residual butyl ester in RB, and washes the resin column with purified water to make the volume of the eluent reach the volume before loading the column 3 times; put the eluate in the reaction tank equipped with penicillin acylase, add boric acid buffer solution according to 10% of the total volume of the degreasing eluent, stir, ...

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Abstract

The invention discloses a process for preparing 6-aminopenicillanic acid, which comprises the following steps: (1) filtering the penicillin fermentation liquid, acidifying, extracting and concentrating with butanol, decoloring to obtain butyl extract of penicillin, (2) subjecting butyl extract of penicillin to back extraction with alkaline solvent, obtaining aqueous solution of penicillin salts, (3) degreasing the aqueous solution of penicillin salts, (4) loading the degreased aqueous solution of penicillin salts into penicillin acylated enzyme retort for enzyme conversion, charging 6-APA seeds, cultivating quartz, crystallizing and drying.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical raw materials, in particular to a preparation method of 6-aminopenicillin alkanoic acid. Background technique [0002] 6-aminopenicillin alkanoic acid is referred to as 6-APA. With 6-APA as the core, it can be condensed with different side chains to prepare β-lactam semi-synthetic antibiotics. β-lactam semi-synthetic antibiotics are widely used in clinic because of their definite curative effect and less toxic side effects. With the extensive use of a series of β-lactam semi-synthetic antibiotics such as amoxicillin and ampicillin, the market demand for its raw material 6-APA is also rising. [0003] At present, the method for preparing 6-APA generally includes the following steps: a, taking the penicillin fermentation liquid as raw material through filtration, acidification, butanol concentration and extraction to make penicillin butyl ester extract; b, alkalizing the penicillin butyl e...

Claims

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Application Information

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IPC IPC(8): C07D499/04C07D499/42
Inventor 刘广春史美平李秋元马志珺王丽郭洪茹田丹霞李彦平高任龙吴立强张亚男张丽娟王晓心梁裕坎赵振刚李晓红林毅
Owner NORTH CHINA PHARMA GROUP CORP
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