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Method for refining D-cycloserine

A technology of cycloserine and refining method, which is applied in the field of pharmaceuticals, can solve the problems of reducing drug efficacy, affecting treatment effect, waste, etc., and achieve the effect of improving product purity, reducing use cost, and product light transmittance

Inactive Publication Date: 2012-03-21
JINAN CHENGHUI SHUANGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of D-cycloserine mainly adopts fermentation method and synthetic method. The purity of D-cycloserine prepared by these methods is extremely difficult to meet the higher standard requirement of 98%-100.0%, and most of them are around 96%. , because D-cycloserine is a drug stored at -20°C at low temperature, and the storage period is only one year, it is easy to be oxidized or polymerized during the storage period to reduce the content; when the content is reduced, it is easy to reduce the efficacy of the drug, and then affect the treatment Effect
Therefore, because the content of D-cycloserine is easy to decrease clinically, it cannot be stored in large quantities, and its content has been greatly reduced in the last 1-2 months of the storage period, resulting in a large amount of clinically abolished D-cycloserine. Serine, resulting in greater waste

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of refining method step of D-cycloserine of the present invention is:

[0036] ① Prepare 297.4 kg of 15% ammonia water for subsequent use;

[0037] ② Cool the 15% ammonia solution to -5°C with ice brine;

[0038] ③Take 100 kg of D-cycloserine recovered product or crude product and slowly add it to a 15% ammonia solution at -5°C, and stir evenly at a temperature of 0°C to -5°C until completely dissolved to obtain a solution;

[0039] 4. Slowly add 476 kilograms of ethanol to the lysate in step 3., and stir for 30 minutes at 0°C—-5°C;

[0040] ⑤ Add 0.01 kg of 8-hydroxyquinoline to the ethanol-containing solution in step ④, stir for 10 minutes at 0°C—-5°C, filter with a 0.45 μm membrane, and cool the filtrate to -5°C;

[0041] ⑥Add acetic acid to the filtrate in step ⑤, adjust the pH value to 5.5-6.5, stir at -5°C for 30 minutes, centrifuge, and dry the solid under reduced pressure at 30°C-35°C for 5 hours to obtain the fine D-cycloserine 93.3 kg, yield 93.3%, p...

Embodiment 2

[0043] A kind of refining method step of D-cycloserine of the present invention is:

[0044] ① Prepare 171.6 kg of 13% ammonia water for subsequent use;

[0045] ② Cool the 13% ammonia solution to -5°C with ice brine;

[0046] ③Take 50 kg of recovered D-cycloserine or crude product and slowly add it to 13% ammonia solution at 0°C, and stir evenly until completely dissolved at a temperature of 0°C--5°C to obtain a solution;

[0047] 4. Slowly add 275 kilograms of ethanol to the solution of step 3., and stir for 30 minutes at 0°C--5°C;

[0048] ⑤ Add 0.005 kg of 8-hydroxyquinoline to the ethanol-containing solution in step ④, stir at 0°C--5°C for 10 minutes, filter with a 0.45 μm membrane, and cool the filtrate to -5°C;

[0049] ⑥Add formic acid to the filtrate in step ⑤, adjust the pH value to 5.5-6.5, stir at -5°C for 30 minutes, centrifuge, and dry the solid under reduced pressure at 30°C-35°C for 5 hours to obtain the fine D-cycloserine 46.6 kg, the yield is 93.2%, and th...

Embodiment 3

[0051] A kind of refining method step of D-cycloserine of the present invention is:

[0052] ① Prepare 524.8 kg of 17% ammonia water for subsequent use;

[0053] ② Cool the 17% ammonia solution to -5°C with ice brine;

[0054] ③Take 200 kg of recovered D-cycloserine or crude product and slowly add it to a 17% ammonia solution at -5°C, and stir evenly at a temperature of 0°C to -5°C until completely dissolved to obtain a solution;

[0055] 4. Slowly add 840 kilograms of methyl alcohol to the lysate of step 3., and stir for 30 minutes at 0°C—-5°C;

[0056]⑤ Add 0.02 kg of 8-hydroxyquinoline to the methanol solution in step ④, stir at 0°C--5°C for 10 minutes, filter with a 0.45 μm membrane, and cool the filtrate to -5°C;

[0057] ⑥Add hydrobromic acid to the filtrate in step ⑤, adjust the pH value to 5.5-6.5, stir at -5°C for 30 minutes, centrifuge, and dry the solid under reduced pressure at 30°C-35°C for 5 hours to obtain D-cyclo 185.4 kg of fine serine, with a yield of 92.7...

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Abstract

The invention discloses a method for refining D-cycloserine. The method comprises the following steps of: (1) preparing an ammonia water solution for later use; (2) cooling the ammonia water solution with brine ice; (3) adding D-cycloserine into the ammonia water solution and uniformly stirring till the D-cycloserine is fully dissolved to obtain a dissolved solution; (4) slowly adding alcohol into the solution obtained in the step (3) and stirring for 30 minutes; (5) adding 0.005-0.02 kilogram of 8-hydroxyquinoline into every 100 kilograms of D-cycloserine, adding 8-hydroxyquinoline into the alcohol-containing solution, preserving heat, stirring for 10 minutes, filtering with a film of 0.45 mum, and cooling the filtrate to -5 DEG C; and (6) adding acid into the filtrate obtained in the step (5), adjusting the pH value, stirring, centrifuging, and drying a solid under reduced pressure for 5 hours to obtain refined D-cycloserine. By adopting the method, D-cycloserine which is overdue clinically can be recovered and refined, so that a higher-purity qualified product can be recycled.

Description

technical field [0001] The invention relates to medicines and relates to a method for refining D-cycloserine. Background technique [0002] D-cycloserine belongs to the class of antibiotics and is clinically used to treat the infection of drug-resistant Mycobacterium tuberculosis. At present, the preparation of D-cycloserine mainly adopts fermentation method and synthetic method. The purity of D-cycloserine prepared by these methods is extremely difficult to meet the higher standard requirement of 98%-100.0%, and most of them are around 96%. , because D-cycloserine is a drug stored at -20°C at low temperature, and the storage period is only one year, it is easy to be oxidized or polymerized during the storage period to reduce the content; when the content is reduced, it is easy to reduce the efficacy of the drug, and then affect the treatment Effect. Therefore, because the content of D-cycloserine is easy to decrease clinically, it cannot be stored in large quantities, an...

Claims

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Application Information

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IPC IPC(8): C07D261/04
Inventor 于东海王素兰杨彦军
Owner JINAN CHENGHUI SHUANGDA CHEM
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