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Method of recycling divalproex sodium crystallization mother liquor

A divalproex sodium and crystallization mother liquor technology, applied in the chemical industry, can solve the problems of difficult quality control, low purity, cumbersome operation, etc., and achieve the effects of easy control of the reaction process, simple and easy method, and reduced production cost

Active Publication Date: 2014-03-26
新方正控股发展有限责任公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is: the local concentration of valproic acid and sodium valproate is uneven, so there may be several mixing ratios in the obtained product, the purity of the product is reduced, and the quality is not easy to control
The disadvantages of this method are: the process has high requirements for equipment, which is difficult to meet in general production, and it is easy to cause product agglomeration during the drying process, affecting the use of the product, and the quality is not easy to control
However, the method is cumbersome to operate, the recovery rate is low, and the quality of recovered divalproex sodium is not up to standard or the purity is not high, which can neither effectively utilize it, but also increase the actual production cost

Method used

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  • Method of recycling divalproex sodium crystallization mother liquor

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Embodiment approach

[0044] A preferred embodiment of the present invention is:

[0045] A method for reclaiming divalproex sodium crystallization mother liquor, comprising:

[0046] 1) Distilling divalproex sodium crystallization mother liquor to obtain a solid mixture containing divalproex sodium;

[0047] 2) adding hydrochloric acid solution to the solid mixture obtained in step 1) to control the pH at 0.5-4.5; and

[0048] 3) Fractional distillation of the organic layer obtained after the reaction in step 2) to obtain valproic acid.

[0049] A more preferred embodiment of the present invention is:

[0050] 1) Concentrate the divalproex sodium reaction mother liquor to dryness;

[0051] 2) Add 10-20% (w / v) concentration of hydrochloric acid until the mother liquor residue is stirred and fully dissolved;

[0052] 3) Stand still and separate the valproic acid layer; and

[0053] 4) Collect the fraction at 112-114℃ / 7~8mmHg under reduced pressure.

[0054] The content of the present invention i...

Embodiment 1

[0059] In a three-neck flask, add divalproex sodium acetone reaction mother liquor 1700ml, recover acetone by atmospheric distillation, and the distillation is completed at 60°C. The concentrated residue weighs about 75 grams, and 15% (w / v) hydrochloric acid solution is added for about 70ml, dissolve all the residue in the stirring bottle, adjust the pH to 1.5, let stand for stratification, distill the upper organic layer under reduced pressure, collect the distillate at 112-114℃ / 7~8mmHg, and obtain 66.2g of valproic acid transparent liquid , the purity measured by gas chromatography was 99.5%, and the yield was 95.0%.

Embodiment 2

[0061] In a three-necked flask, add divalproex sodium acetone reaction mother liquor 1700ml, recover acetone by atmospheric distillation, and the distillation is completed at 60°C. The concentrated residue weighs about 75 grams, and 10% (w / v) hydrochloric acid solution is added for about 110ml, dissolve all the residue in the stirring bottle, adjust the pH to 0.5, let it stand for stratification, distill the upper organic layer under reduced pressure, collect the distillate at 112-114℃ / 7~8mmHg, and obtain 66.3 grams of valproic acid transparent liquid , the purity measured by gas chromatography was 99.6%, and the yield was 95.2%.

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Abstract

The invention provides a method of recycling divalproex sodium crystallization mother liquor. The method comprises the following steps: (1), concentrating the divalproex sodium crystallization mother liquor to obtain a solid-state mixture containing divalproex sodium; (2), carrying out acidizing treatment onto the solid-state mixture obtained in the step (1), controlling pH to 0.5-4.5 to obtain an organic layer; and (3), carrying out fractionation onto the organic layer obtained in the step (2) to obtain valproic acid. Yield of the valproic acid obtained by the method disclosed by the invention can be as high as 95%, and purity of the valproic acid is not lower than 99.1%, so that medicinal requirements can be satisfied. Moreover, the method disclosed by the invention is simple and easy to implement and easy to control in a reaction process, lowers actual production cost, and satisfies large-scale industrial production requirements.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for recycling divalproex sodium crystallization mother liquor. Background technique [0002] Divalproex sodium is an anticonvulsant and mood stabilizing drug mainly used in the treatment of epilepsy and bipolar disorder, and can also be used in the treatment of migraine and schizophrenia. Divalproex sodium is used to control absence seizures, tonic-clonic seizures (grand mal), complex partial seizures, and seizures associated with Lennox-Gastaut syndrome in patients with epilepsy. Divalproex binds and inhibits GABA transaminase. It acts by dissociation into valproate ions in the gastrointestinal tract. Divalproex sodium has less gastrointestinal side effects and fewer drug interactions, so it has physiological properties equal to or better than valproic acid or sodium valproate, and is widely used clinically. [0003] The report about the synthetic techniq...

Claims

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Application Information

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IPC IPC(8): C07C53/128C07C51/02
CPCC07C51/02C07C53/128
Inventor 张小均马德银赵德贺清凯刘永红
Owner 新方正控股发展有限责任公司
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