Method for preparing divalproex sodium

A technology of divalproex sodium and valproic acid, which is applied in carboxylate preparation, organic chemistry, etc., can solve the problems such as the purity of divalproex sodium and achieve excellent fluidity, low cost and short cycle Effect

Active Publication Date: 2013-07-03
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In addition, in this patent document, there is no mention of the purity of the obtained divalproex sodium

Method used

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  • Method for preparing divalproex sodium
  • Method for preparing divalproex sodium

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Effect test

Embodiment 1

[0051]

[0052] At room temperature, in 1000ml four-neck flask, add 750ml acetone, 73.7g (0.512mol, 1.0eq (molar equivalent)) valproic acid, then add 10.4g (0.26mol, 0.5eq) sodium hydroxide solid, stir until solid The mixture was completely dissolved, and the mixed system was frozen and crystallized at -15°C overnight, and then the obtained solid was filtered with suction, and the filter cake was washed with a small amount of cold acetone to obtain 75.1 g of a white solid with a yield of 95% and an HPLC purity of 99.86 %.

[0053] HNMR (CDCl 3 , ppm): δ13.16 (brs, 1H), 2.25-2.19 (m, 2H), 1.45-1.57 (m, 4H), 1.21-1.39 (m, 12H), 0.86 (t, J=7.2Hz, 12H ).

Embodiment 2

[0055] At room temperature, in 1000ml four-neck flask, add 600ml acetone, 37.9g ​​(0.263mol, 1.0eq) valproic acid, then add 5.3g (0.13mol, 0.5eq) sodium hydroxide solid, stir until the solid is completely dissolved, and The mixed system was frozen and crystallized at -12°C overnight, and then the obtained solid was suction-filtered, and the filter cake was washed with a small amount of cold acetone to obtain 38.0 g of a white solid with a yield of 93.2% and an HPLC purity of 99.15%.

Embodiment 3

[0057] At room temperature, in the 1500ml four-necked flask, add the mixed solution of 850ml acetone and acetonitrile (acetone: acetonitrile=3:1 (V / V)) and 71.6g (0.497mol, 1.0eq) valproic acid, then add 9.9g (0.25mol, 0.5eq) sodium hydroxide solid, stirred until the solid was completely dissolved, placed the mixed system at -5°C for freezing and crystallization overnight, then suction filtered the resulting solid, and washed the filter cake with a small amount of cold acetone to obtain 66g white solid, yield 85.6%, HPLC purity 99.03%.

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Abstract

The invention provides a method for preparing divalproex sodium. The method comprises: (1) reacting valproic acid with sodium hydroxide in an organic solvent, to obtain divalproex sodium, wherein the organic solvent may be acetone and/or acetonitrile; and (2) precipitating, under -20-30 DEG C, divalproex sodium made in the step (1) from the organic solvent, thereby obtaining a divalproex sodium crystal. The method for preparing divalproex sodium in the invention has advantages of stable properties and high yield, the HPLC purity reaches higher than 99%, and the method of the invention is suitable for large scale industrialization production.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and in particular relates to a method for preparing divalproex sodium. Background technique [0002] Divalproex sodium, also known as semi-sodium valproate, was first developed and marketed by Abbott Laboratories of the United States in April 1983. It is an anticonvulsant drug and a mood-stabilizing drug, which is mainly used for the treatment of epilepsy and bipolar emotion disorder, and can also be used to treat migraines and schizophrenia. Divalproex sodium can be used to control absence seizures, tonic-clonic seizures (grand mal seizures), complex partial seizures, and seizures associated with Lennox-Gastaut syndrome in patients with epilepsy. Divalproex sodium dissociates into valproate ions in the gastrointestinal tract, which acts by binding to and inhibiting GABA transaminase. [0003] US4,988,731 and US5,212,326 disclose semisodium valproate (INN: Valproate semisodium, CAS: 76584-70-8, US...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/128C07C51/41
Inventor 陶晶林松文钟学超邓小兵
Owner NEW FOUNDER HLDG DEV LLC
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