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Method for recovering 2-propylmalonic acid and preparing valproic acid from 2-propylmalonic acid

A technology of propylmalonic acid and dipropylmalonic acid, which is applied to the recovery of 2-propylmalonic acid and the field of preparing valproic acid, can solve the problem of increasing the difficulty of wastewater treatment, increasing the oxygen consumption value of wastewater, Increase the manufacturing cost and other issues to achieve the effect of reducing the difficulty of processing, reducing chemical oxygen consumption and saving costs

Active Publication Date: 2020-12-29
湖南省湘中制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It not only reduces the total yield, but also increases the manufacturing cost. The presence of these organic acids also increases the oxygen consumption value of the wastewater and increases the difficulty of wastewater treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Pump 1,000 kg of acidic water after centrifugal separation of 2,2-dipropylmalonic acid into a 2,000-L reactor, add 250 kg of tert-butyl methyl ether while stirring, continue stirring for 1 hour, and let stand to separate layers. Dry over anhydrous magnesium sulfate, filter, put the filtrate into a clean and dry esterification kettle, concentrate to dryness, add 400kg of absolute ethanol, 5kg of concentrated sulfuric acid for reaction, after the reaction is complete, post-treatment to obtain diethyl 2-propylmalonate. Then add 2.5kg of sodium ethylate to catalyze propylation, hydrolysis, acidification and separation, and decarboxylation. Get valproic acid 14.2kg. The content (GC) is 99.8%.

Embodiment 2

[0019] Pump 1000kg of acidic water after centrifugal separation of 2,2-dipropylmalonic acid into a 2000L reaction kettle, add 250kg of ethyl acetate under stirring, continue stirring for 1 hour, and let stand to separate layers. Dry over anhydrous magnesium sulfate, filter, put the filtrate into a clean and dry esterification kettle, concentrate to dryness, add 400kg of absolute ethanol, 5kg of concentrated sulfuric acid for reaction, after the reaction is complete, post-treatment to obtain diethyl 2-propylmalonate. Then add 2.5kg of sodium ethylate to catalyze propylation, hydrolysis, acidification and separation, and decarboxylation. Get valproic acid 12.3kg. The content (GC) is 99.6%.

Embodiment 3

[0021] Pump 1,000 kg of acidic water after centrifugal separation of 2,2-dipropylmalonic acid into a 2,000 L reactor, add 250 kg of n-butanol under stirring, continue stirring for 1 hour, and let stand to separate layers. Dry over anhydrous magnesium sulfate, filter, put the filtrate into a clean and dry esterification kettle, concentrate to dryness, add 400kg of absolute ethanol, 5kg of concentrated sulfuric acid for reaction, after the reaction is complete, post-treatment to obtain diethyl 2-propylmalonate. Then add 2.5kg of sodium ethylate to catalyze propylation, hydrolysis, acidification and separation, and decarboxylation. Get valproic acid 14.3kg. The content (GC) is 99.7%.

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Abstract

The invention discloses a method for recovering 2-propylmalonic acid and preparing valproic acid from 2-propylmalonic acid, and the method for recovering 2-propylmalonic acid and preparing valproic acid from 2-propylmalonic acid includes the following steps: (1) collecting acid water after centrifuging dipropylmalonic acid, adding ether, ester, chlorinated hydrocarbon and an alcohol (immiscible with water) solvent, stirring, extracting, layering, and drying to obtain dipropylmalonic acid with the recovery rate of more than 90%; and (2) performing esterification, propylation, hydrolysis and acidification on the 2-propylmalonic acid to obtain dipropylmalonic acid, and performing decarboxylation to obtain high-purity valproic acid (the content is greater than or equal to 99.5%). Through recovery and comprehensive utilization of the 2-propylmalonic acid, the production cost of the 2-propylvaleric acid is reduced, and the pressure of subsequent environmental protection treatment is greatlyreduced.

Description

technical field [0001] The invention relates to recovery of 2-propylmalonic acid and a method for preparing valproic acid. Background technique [0002] 2-Propylvaleric acid and its derivatives belong to the first-line antiepileptic drugs, which act in the form of valproic acid after being absorbed by the body. seizures, partial motor seizures, absence seizures, and infantile spasms. Today, the therapeutic field of valproic acid and its derivatives is still expanding. In addition to anti-epilepsy, the FDA-approved indications also include bipolar disorder and migraine. [0003] The method of obtaining valproic acid through propylation, hydrolysis, acidification and decarboxylation of diethyl malonate has become the first choice for large-scale industrial production of valproic acid and its derivatives by many manufacturers. However, according to analysis and statistics, after acidification and separation of 2,2-dipropylmalonic acid, the acid water contains more organic aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/38C07C53/126C07C51/09C07C55/02C07C67/08C07C67/343C07C69/34
CPCC07C51/38C07C51/09C07C67/08C07C67/343C07C69/34C07C55/02C07C53/126
Inventor 段世辉杨贞皓彭辉
Owner 湖南省湘中制药有限公司
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