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Oxiracetam compound and new method thereof

A compound, separation and purification technology, applied in the medical field, can solve the problems of insufficient purity, no public purification of oxiracetam compounds, etc., to achieve the effect of improving purity and content, simple and easy process, and ensuring safety

Inactive Publication Date: 2011-05-11
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] CN101367757A, CN101575309A, CN101121688A, CN101693685A, CN1948285A disclosed the synthesis route of the process, but the purity still cannot meet the requirements of clinical medicine, and further refining treatment is required
[0014] For these impure products, the prior art does not disclose the method for purifying oxiracetam compounds. In fact, those skilled in the art with general experience clearly know the various difficulties faced in obtaining high-purity compounds, all of which are by no means The existing general separation and purification theory can be expected to be solved, and many difficulties need to be overcome

Method used

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  • Oxiracetam compound and new method thereof
  • Oxiracetam compound and new method thereof
  • Oxiracetam compound and new method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 The refining of oxiracetam

[0038] (1) Dissolve 100 g of crude oxiracetam with a purity of 96.7% in 1000 ml of purified water, add 2 g of activated carbon, stir at 60° C. for 20 min, filter for decarburization, and collect the filtrate;

[0039] (2) in gained filtrate, slowly add the mixed solvent 3000ml that volume ratio is the acetonitrile and isopropyl ether of 2: 1, stir, produce precipitation, filter and obtain oxiracetam solid;

[0040] (3) put oxiracetam solid on the column, separate and purify by chromatographic column, with the acetonitrile and water mixed solvent of volume ratio 1: 3 as mobile phase, stationary phase filler is aluminum oxide, flow velocity is 3.0ml / min, column temperature 30°C, collect the fractions in sections, and combine the eluents with a content greater than 90%;

[0041] (4) Concentrate the eluent under reduced pressure to about 1 / 2 volume, add 1000ml of acetonitrile and isopropyl ether mixed solvent with a volume ratio of 2:...

Embodiment 2

[0042] Example 2 The refining of oxiracetam

[0043] (1) Dissolve 100 g of crude oxiracetam with a purity of 96.7% in 1000 ml of purified water, add 5 g of activated carbon, stir at 50° C. for 30 min, filter for decarburization, and collect the filtrate;

[0044] (2) in gained filtrate, slowly add the mixed solvent 6000ml that volume ratio is 2: 1 acetonitrile and isopropyl ether, stir, produce precipitation, filter to obtain oxiracetam solid;

[0045] (3) put oxiracetam solid on the column, separate and purify by chromatographic column, be mobile phase with the mixed solvent of acetonitrile and water of 1: 3 with the volume ratio, stationary phase filler is aluminum oxide, flow velocity is 5.0ml / min, column Warm at 40°C, collect the fractions in sections, and combine the eluents with a content greater than 90%;

[0046] (4) Concentrate the eluent under reduced pressure to about 1 / 2 volume, add 1000 ml of acetonitrile and isopropyl ether mixed solvent with a volume ratio of 2...

Embodiment 3

[0047] Example 3 The purification of oxiracetam

[0048] (1) Dissolve 100 g of crude oxiracetam with a purity of 96.7% in 1000 ml of purified water, add 3 g of activated carbon, stir at 60° C. for 30 min, filter for decarburization, and collect the filtrate;

[0049] (2) in the obtained filtrate, slowly add the mixed solvent 4000ml of acetonitrile and isopropyl ether with a volume ratio of 2: 1, stir to produce precipitation, filter to obtain the oxiracetam solid;

[0050] (3) put oxiracetam solid on the column, separate and purify by chromatographic column, be mobile phase with the mixed solvent of acetonitrile and water of 1: 3 with the volume ratio, stationary phase filler is aluminum oxide, flow velocity is 2.5ml / min, column Warm at 25°C, collect the fractions in sections, and combine the eluents with a content greater than 90%;

[0051] (4) Concentrate the eluent under reduced pressure to about 1 / 2 volume, add 1000 ml of acetonitrile and isopropyl ether mixed solvent wit...

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Abstract

The invention provides an Oxiracetam compound and a new method thereof. The method comprises the following steps: firstly dissolving Oxiracetam in water, carrying out adsorption and purification with activated carbon, precipitating with an organic solvent, separating and purifying with a chromatographic column, and finally carrying out crystallization with an organic solvent, thus the high purity Oxiracetam compound is obtained. The purity of the final product is greatly improved compared with the existing product, the quality of preparation is improved, the toxic and side effects are reduced, and the safety in the application of preparing a drug used for treating senile dementia is ensured; and meanwhile, compared with the prior art, the process in the invention is simple and feasible, the reaction conditions are mild, the cost is low, the yield is high, and the product purity is high, thus being applicable to industrialized production.

Description

technical field [0001] The invention relates to an oxiracetam compound and a new method thereof, belonging to the technical field of medicine. Background technique [0002] Nootropics, also known as cereboactive drugs, are a new class of central nervous system drugs that can promote learning and memory. They can selectively act on the cerebral cortex and hippocampus to activate, protect or promote the development of nerve cells. Functional recovery, while the drug itself has no direct vasoactive or central stimulating effect, and its effect on learning and memory is a lasting promotion effect. These compounds are all γ-aminobutyric acid derivatives, such as piracy Tan, Oxiracetam, and Nefiracetam. At present, this type of drug has attracted widespread attention and interest, and the demand for this type of drug is also increasing day by day. [0003] Oxiracetam is a synthetic cyclic derivative of carboxyaminobutyric acid (GABOB), chemically named 2-[4-hydroxypyrrolidin-2-o...

Claims

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Application Information

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IPC IPC(8): C07D207/273A61P25/28
Inventor 王明
Owner HAINAN LINGKANG PHARMA CO LTD
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