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Refining method of D-pantolactone

A technology of pantolactone and a refining method, which is applied in the field of D-pantolactone refining, can solve the problem that the optical purity of products cannot meet high-level requirements, the optical purity of D-pantolactone is insufficient, and the environment is unfriendly. and other problems, to achieve the effect of easy operation, large crystal, and saving investment.

Active Publication Date: 2020-03-06
安徽泰格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the existing methods for class separation have the problem of insufficient optical purity of D-pantoolactone, and it is necessary to refine and obtain qualified D-pantoolactone for use
The existing methods for refining D-pantolactone mostly use organic solvents with high toxicity and unfriendly environment, and the optical purity of the obtained products cannot meet the high-level requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The present embodiment provides a kind of refining method of D-pantolactone, and concrete steps are:

[0019] (1) Add 20g of 95% ethyl acetate in turn to a clean 500ml one-mouth bottle, with a specific rotation of +40°D-pantolactone 100g, stir evenly, heat up to 70°C to dissolve, add 0.5g of activated carbon to filter , the filtrate began to stir and cool down to 20°C, then added 0.5g of qualified D-pantolactone, and then began to slowly cool down to 10°C with a gradient. After 4 hours of heat preservation and crystallization, 56g of material was obtained by filtration, white crystalline particles, and the specific rotation was 49.6°. Loss on drying 1.8%;

[0020] (2) Add 0.5g of D-pantolactone to the mother liquor after filtration, then continue to cool down to -5°C, heat and crystallize for 4 hours, and then filter to obtain 26g of the material, white crystalline particles, with a specific rotation of 49.9°, a loss on drying of 2.1%, and a yield of About 80-82%;

[...

Embodiment 2

[0023] The present embodiment provides a kind of refining method of D-pantolactone, and concrete steps are:

[0024] (1) To a clean 500ml one-mouth bottle, add 20g of 90% ethyl acetate in turn, with a specific rotation of +40°D-pantolactone 100g, stir evenly, heat up to 70°C to dissolve, then add 0.5g of activated carbon Filtrate, stir and cool the filtrate to 20°C, then add 0.5g of qualified D-pantolactone, then gradually cool down to 10°C, keep warm and crystallize for 4 hours, and then filter to obtain 45g of the material, white crystal particles, with a specific rotation of 50.1° , loss on drying 1.8%;

[0025] (2) Add 0.5g of D-pantolactone to the mother liquor after filtration, continue to cool down to -5°C, heat and crystallize for 4h, and then filter to obtain 15g of material, white crystalline particles, specific rotation is 50.5°, and loss on drying is 1.9%. The rate is about 60-62%;

[0026] (3) After recovering the ethyl acetate from the mother liquor, return to ...

Embodiment 3

[0028] The present embodiment provides a kind of refining method of D-pantolactone, and concrete steps are:

[0029] (1) To a clean 500ml single-necked bottle, add 30g of 95% ethyl acetate in turn, with a specific rotation of +40°D-pantolactone 100g, stir evenly, heat up to 70°C, dissolve and add 0.5g Activated carbon filtration, the filtrate began to stir and cool down to 20°C, then added 0.5g of qualified D-pantolactone, then began to gradually cool down to 10°C, kept warm and crystallized for 4 hours, and filtered to obtain 46g of the material, white crystal particles, with a specific rotation of 49.9 °, loss on drying 1.8%;

[0030] (2) Add 0.5g of D-pantolactone to the mother liquor after filtration, then continue to cool down to -5°C, heat and crystallize for 4 hours, and then filter to obtain 20g of the material, white crystalline particles, with a specific rotation of 50.2° and a loss on drying of 2.0%. The yield is about 65-67%;

[0031] (3) After recovering the eth...

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Abstract

The invention relates to a refining method of D-pantolactone. The method comprises the following steps: mixing a D-pantolactone crude product with the specific rotation of more than -45.0 degrees withethyl acetate, heating and fully dissolving, controlling the temperature at 20-30 DEG C, adding a D-pantolactone seed crystal with the specific rotation of -45.0 degrees to -50.7 degrees, slowly cooling to 5-10 DEG C, carrying out heat preservation crystallization, filtering, and collecting the crystal. The refining method of the D-pantolactone has the advantages that the raw materials are easy to obtain, the conditions are environmentally friendly and safe, the reaction time is short, the solvent can be recycled, the steps are simple, the obtained product is large and uniform in crystal, thespecific rotation can reach -49.5 degrees to -50.5 degrees, the purity can reach 98.0%, and the refining method has extremely high industrial utilization value.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to a method for refining D-pantolactone. Background technique [0002] D-pantolactone is an organic chemical that can be obtained by chiral resolution of DL-pantoolactone. D-pantothenolactone is mostly used in the synthesis of D-panthenol, D-calcium pantothenate, D-panthenol ethyl ether, etc. [0003] The prior art provides a variety of resolution methods for DL-pantolactone. For example, Fusarium oxysporum is cultured in the culture medium, and the cultured Fusarium oxysporum is mixed with the substrate, hydrolyzed to obtain D-pantoic acid, and lactonized to obtain D-pantoic acid lactone. For another example, use a chiral reagent to form a double salt with DL-pantolactone, use the different solubility of the double salt in the solvent, separate the double salt of the D-body and the L-body, and then obtain the D- The body of pantoate lactone, and then recovery of L-body pantoat...

Claims

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Application Information

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IPC IPC(8): C07D307/33
CPCC07D307/33C07B2200/13
Inventor 蔡奇峰汪洪湖段小瑞祁翔谢伟
Owner 安徽泰格生物科技有限公司
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