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Method for continuously crystallizing 6-amino-penicillanic acid

A technology of crystallization of aminopenicillanic acid, which is applied in the field of medicine, can solve problems such as the inability to realize automatic control, increase the cost of production enterprises, and unstable product quality, and achieve the effect of ensuring uniformity, reducing waste of resources, and good uniformity

Active Publication Date: 2015-06-24
INNER MONGOLIA CHANGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This staged phase separation and crystallization operation is intermittent, which will lead to unstable product quality and large batch-to-batch differences, and the intermittent operation cannot realize automatic control, which requires a lot of manpower and increases the cost of production enterprises.

Method used

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  • Method for continuously crystallizing 6-amino-penicillanic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The volume of the reaction tank is 100L, the set height of the liquid level in the reaction tank is 60% of the height of the reaction tank, and the bottom end of the stirring paddle is located at 2 / 3 of the set liquid level.

[0035] The volume of the crystallization tank is 100L, and the set height of the liquid level in the crystallization tank is 60% of the height of the crystallization tank.

[0036] There are five sets of filtering devices.

[0037] a. The lysate with a 6-APA content of 22% is continuously fed into the pipeline mixer at a constant flow rate of 20 L / min, and at the same time, butanol is continuously fed into the pipeline mixer at a constant speed of 4 L / min , the two are mixed to obtain a mixed solution;

[0038] b. Control the temperature of the reaction tank at 10°C, turn on the stirring, and continuously pass the mixed solution in the pipeline mixer into the reaction tank at a constant flow rate of 24L / min, and at the same time, add 20% hydrochl...

Embodiment 2

[0044] The volume of the reaction tank is 100L, the height of the liquid level in the setting reaction tank is 80% of the height of the reaction tank, and the bottom end of the stirring paddle is located at 1 / 2 of the setting liquid level.

[0045] The volume of the crystallization tank is 100L, and the set height of the liquid level in the crystallization tank is 80% of the height of the crystallization tank.

[0046] There are three sets of filtering devices.

[0047] a. The lysate with a 6-APA content of 28% is continuously fed into the pipeline mixer at a constant flow rate of 30 L / min, and at the same time, butanol is continuously fed into the pipeline mixer at a constant speed of 6 L / min , the two are mixed to obtain a mixed solution;

[0048] b. The temperature of the reaction tank is controlled at 5°C, the stirring is turned on, and the mixed solution in the pipeline mixer is continuously passed into the reaction tank at a constant flow rate of 36L / min, and 20% aqueou...

Embodiment 3

[0054] The inventor has carried out quality detection to the 6-aminopenicillanic acid that embodiment 1-2 obtains, and the result is shown in table 1, table 2.

[0055] Table 1

[0056] sample

content

simple

total miscellaneous

color grade

moisture

Example 1-1

99.5％

0.21％

0.53％

2#

0.3％

Example 1-2

99.4％

0.32％

0.54％

2#

0.3％

Example 1-3

99.3％

0.31％

0.51％

2#

0.2％

Example 1-4

99.5％

0.24％

0.49％

2#

0.2％

Example 1-5

99.2％

0.23％

0.55％

2#

0.3％

[0057] Table 2

[0058] sample

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Abstract

The invention discloses a method for continuously crystallizing 6-amino-penicillanic acid and relates to the technical field of medical intermediate synthesis. The method is used for overcoming the defect of great quality difference between different batches of products obtained by use of an intermittent split-phase crystallization method in the prior art by virtue of a continuous crystallization; and as a result, the uniformity of the products is greatly improved, and meanwhile, the automatic control is applied, the production efficiency is improved and the energy source is saved.

Description

technical field [0001] The invention belongs to the technical field of medicine and relates to a preparation method of a medicine intermediate, in particular to a method for continuous crystallization of 6-aminopenicillanic acid. Background technique [0002] 6-aminopenicillanic acid, referred to as 6-APA, has the following structure: [0003] [0004] 6-APA can introduce different side chains to obtain antibiotics with different drug effects, and is an important intermediate for the production of semi-synthetic penicillin antibiotics ampicillin sodium and amoxicillin. [0005] The traditional preparation process of 6-APA is to use penicillin fermentation liquid as the starting material, after two extractions and phase separation, a degreasing liquid containing penicillinic acid is obtained, which is cleaved by penicillin acylase to obtain a lysate containing 6-APA, Then hydrochloric acid was added for extraction and phase separation, and ammonia water was added to the w...

Claims

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Application Information

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IPC IPC(8): C07D499/18C07D499/42
CPCC07D499/18C07D499/42
Inventor 徐永龙刘健郭军臣袁国强王永伟赵英杰梅玉龙
Owner INNER MONGOLIA CHANGSHENG PHARMA
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