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Method for refining oxiracetam

A refining method and crude product technology, applied in the direction of organic chemistry, can solve the problems of many by-products and low product quality, and achieve the effects of low cost, simple operation, and easy recycling

Active Publication Date: 2012-05-02
SHANDONG JINHE DRUG RES DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the deficiencies in the prior art, especially the problems that there are many by-products and low product quality in the oxiracetam products currently on the market, the invention provides a method for refining oxiracetam to obtain a purity of more than 99.9% (total impurity less than 0.1%) oxiracetam boutique

Method used

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  • Method for refining oxiracetam
  • Method for refining oxiracetam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1, batching ratio: oxiracetam crude product: absolute ethanol: phosphoric acid: glacial acetic acid=1: 25: 0.01: 0.5.

[0033] The refining method of oxiracetam comprises steps as follows:

[0034] 1. Add 12.5L of absolute ethanol, 5ml of phosphoric acid, and 250ml of glacial acetic acid into a 20L three-necked flask in sequence, start stirring, and heat the water bath to 60°C±2°C.

[0035] 2. Add 500g of ground crude oxiracetam into the above reaction flask, stir and raise the temperature to 80°C±2°C for reflux, keep reflux at this temperature for 30min to fully dissolve it, then add 5g of activated carbon, stir, and keep reflux Temperature, continue to reflux for 20min.

[0036] 3. Turn off the heating of the water bath, filter the reaction solution while it is hot to obtain a colorless and clear solution, pour the solution into another clean 20L reaction bottle, stir, and circulate the ice and salt water to naturally cool the solution in the reaction bott...

Embodiment 2

[0039] Embodiment 2, ingredient ratio: oxiracetam crude product: absolute ethanol: phosphoric acid: glacial acetic acid=1: 27: 0.02: 0.7.

[0040] The refining method of oxiracetam, as described in embodiment 1, the difference is:

[0041] Add 13.5L of absolute ethanol, 10ml of phosphoric acid, and 350ml of glacial acetic acid into a 20L three-necked flask in sequence, start stirring, and heat the water bath to 60°C±2°C. The rest of the steps, dosage and conditions were the same as in Example 1 to obtain 402 g of oxiracetam fine product; the purity was 99.929%, the maximum single impurity was 0.033%, the total impurity was 0.071%, and the yield was 80.4%.

Embodiment 3

[0042] Embodiment 3, ingredient ratio: oxiracetam crude product: absolute ethanol: phosphoric acid: glacial acetic acid=1: 30: 0.05: 0.9.

[0043] 1. Add 15.0L of absolute ethanol, 25ml of phosphoric acid, and 450ml of glacial acetic acid into a 20L three-necked flask in sequence, start stirring, and heat the water bath to 60°C±2°C.

[0044] 2. Add 500g of ground crude oxiracetam to the above reaction flask, stir and heat up to 80°C±2°C for reflux, keep reflux at this temperature for 28min to fully dissolve it, then add 5g of activated carbon, stir and keep the temperature , continue to reflux for 20min.

[0045] 3. Turn off the heating of the water bath, and filter the reaction solution while it is hot to obtain a colorless and clear solution. Pour the solution into another clean 20L reaction bottle, stir, and circulate the ice-salt water to cool it down to 5-10°C naturally. Crystal 11h, crystallization is sufficient.

[0046] 4. Put the material into the centrifuge for centr...

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Abstract

The invention relates to a method for refining oxiracetam, which comprises the following steps: adding a crude oxiracetam product into a mixed solvent of anhydrous alcohol, phosphoric acid and glacial acetic acid, heating to 80+ / -2 DEG C under reflux, adding activated carbon and continuing reflux; and filtering while the solution is hot to obtain a colorless clear solution, stirring at 5-10 DEG Cto crystallize for 10-12 hours, centrifugalizing, and drying to obtain the fine oxiracetam product. The purity of the fine oxiracetam product is higher than 99.9%, the maximum single impurity contentis less than 0.05%, and the total impurity content is less than 0.1%. The invention is simple to operate, environment-friendly, and applicable to industrial mass production.

Description

field of invention [0001] The invention relates to a method for refining oxiracetam, a medicine for improving brain metabolism. Background technique [0002] Oxiracetam, the chemical name is 4-hydroxy-2-oxo-1-pyrrolidineacetamide, the English name is Oxiracetam, and the structural formula is as follows: [0003] [0004] The trade name is Naofuzhi, which is a drug for improving brain metabolism and belongs to the cyclic derivative of γ-aminobutyric acid. It can promote the synthesis of ATP and acetylcholine in the brain, resist brain function damage caused by physical and chemical factors and promote brain metabolism, and can improve retrograde amnesia caused by hypoxia. Can enhance memory and improve learning ability. Oxiracetam was synthesized for the first time in 1977 by the Italian I.S.F company [US4118396], and it went on the market in 1984. Oxiracetandol currently on the market exists in the form of its racemate. For the preparation method of oxiracetam, see US...

Claims

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Application Information

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IPC IPC(8): C07D207/273
Inventor 常建晖张义智王振高英涵彭坤
Owner SHANDONG JINHE DRUG RES DEV
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