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Oxiracetam refining and purifying method

A technology for refining and refining products, applied in the field of purification, can solve problems such as difficult to meet preparation requirements, high cost, complicated operation, etc., and achieve the effect of being suitable for large-scale industrial production, mild conditions, and simple operation

Active Publication Date: 2015-06-03
QINGDAO HUANGHAI PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing methods may not be able to obtain a product with a purity of more than 99.0%, which is difficult to meet the requirements of the preparation, or use water as a solvent to reduce the product yield, or the operation is complicated, such as refining by column chromatography, which is difficult to achieve in production, or The use of mixed solvents makes the solvents unable to be recycled and used mechanically, resulting in high costs

Method used

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  • Oxiracetam refining and purifying method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2.3kg of crude oxiracetam to 23kg of methanol, reflux at 70°C for 1 hour to dissolve, add 2.3kg of activated carbon, continue to reflux at 70°C for 0.5h, and filter while hot at 65°C to obtain a light yellow transparent filtrate, 2.3kg of hot methanol at 60°C Wash the filter cake; combine the washing solution and the filtrate, concentrate under reduced pressure at 40°C, stop concentrating when 11.5L remains, cool down to -2°C for crystallization for 6 hours, filter, and wash the filter cake with ice methanol at 0°C to obtain off-white crystals 1.65kg primary refined product of oxiracetam; add 1.65kg primary refined product of oxiracetam to 16.5kg methanol, heat to reflux for 1h to dissolve, add 1.65kg of activated carbon, continue to reflux at 70°C for 0.5h, filter while hot at 65°C , to obtain a colorless and transparent filtrate, 1.65 kg of hot methanol at 60°C to wash the filter cake; after combining the washing liquid and the filtrate, concentrate under reduced p...

Embodiment 2

[0021] Add 1.5kg of crude oxiracetam to 15kg of methanol, reflux at 70°C for 1 hour to dissolve, add 0.75kg of activated carbon, continue to reflux at 70°C for 0.5h, and filter while hot at 60°C to obtain a light yellow transparent filtrate, 1.5kg of hot methanol at 65°C Wash the filter cake; combine the washing liquid and the filtrate, concentrate under reduced pressure at 40°C, stop the concentration when 7.5L remains, cool down to -3°C for crystallization for 8 hours, filter, wash the filter cake with ice methanol at 0°C, and obtain off-white crystals 1.0kg primary refined product of oxiracetam; add 1.0kg primary refined product of oxiracetam to 10.0kg methanol, heat to reflux for 1 hour to dissolve, add 0.5kg of activated carbon, continue to reflux at 70°C for 0.5h, filter while hot at 60°C , to obtain a colorless and transparent filtrate, 1.0kg of 65°C hot methanol to wash the filter cake; after combining the washing liquid and the filtrate, concentrate under reduced press...

Embodiment 3

[0023] Add 1.2kg of crude oxiracetam to 12kg of recovered methanol, reflux at 70°C for 1 hour to dissolve, add 0.6kg of activated carbon, continue to reflux at 70°C for 0.5h, and filter while hot at 63°C to obtain a light yellow transparent filtrate, 1.2kg 62°C Heat recovered methanol to wash the filter cake; after combining the washing liquid and the filtrate, concentrate under reduced pressure at 40°C, stop concentrating when 6.0L remains, cool down to -2°C for crystallization for 8 hours, filter, and wash the filter cake with ice-recovered methanol at 0°C. Obtain 0.93 kg of the primary refined product of off-white crystal oxiracetam; add 0.93 kg of the primary refined product of oxiracetam to 9.3 kg of recovered methanol, heat to reflux for 1 hour to dissolve, add 0.47 kg of activated carbon, and continue to reflux at 70 ° C for 0.5 h. Filtrate while hot at 63°C to obtain a colorless transparent filtrate, wash the filter cake with 0.93kg methanol at 62°C heat recovery; combi...

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Abstract

The invention relates to a purification method and in particular relates to an oxiracetam refining and purifying method. The method comprises the following steps: adding crude oxiracetam into methanol for refluxing and dissolving, adding activated carbon after dissolving, and continuously refluxing at the refluxing and dissolving temperature for 0.5-2 hours; filtering while hot, flushing the filter cake by using hot methanol, mixing the scrubbing solution and a filtrate, performing vacuum concentration, and separating out a white crystal, namely a primary oxiracetam refined product while stirring at the temperature of 5 DEG C below zero to 0 DEG C, so that the crude oxiracetam is refined; and adding the primary oxiracetam refined product into methanol again, performing repeated refining treatment, thereby obtaining the oxiracetam of which the purity is over 99 percent and the content of single impurity is less than 0.1 percent. The method disclosed by the invention is mild in conditions, easy to operate and low in cost and is suitable for large-scale industrial production, and the solvent can be recycled.

Description

technical field [0001] The invention relates to a purification method, in particular to a method for refining and purifying oxiracetam. Background technique [0002] Oxiracetam (4-hydroxy-2-oxo-1-pyrrolidineacetamide) is a nootropic drug that acts on the cholinergic brainstem reticular structure. Synthetic, listed in Italy in 1987. Its structure is as follows: [0003] [0004] Oxiracetam can selectively act on the cerebral cortex and hippocampus to activate, protect or promote the functional recovery of nerve cells, but it has no direct vascular activity and no central excitatory effect. It is a long-lasting effect on the improvement of learning and memory ability. enhancement. Oxiracetam only acts on the central nervous system, which can improve brain metabolism, enhance and promote the intelligence of young people, improve brain dysfunction and memory impairment in the elderly, and treat neurosis and mental behavioral disorders, especially Alzheimer's disease. It c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/273
CPCC07D207/273
Inventor 张姗李常青鲁大东陈晓涛王宝超刘志达高永吉
Owner QINGDAO HUANGHAI PHARM CO LTD