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Preparation method of high-purity amantadine hydrochloride

A high-purity technology of amantadine hydrochloride, which is applied in the fields of purification/separation of amino compounds, organic chemistry, etc., can solve the problems of difficulty, low impurity removal efficiency, and high preparation cost

Pending Publication Date: 2020-11-20
中涛新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although in the production control, it is completely feasible to meet the pharmaceutical quality standards, it is difficult to prepare some higher-purity amantadine hydrochloride for special purposes. Multiple recrystallizations and low impurity removal efficiency lead to high preparation costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] S1 extraction, the materials reacted in the process of producing amantadine hydrochloride are extracted by extraction oil and then left to stand for stratification;

[0023] S2 is washed with water, and after the stratification is completed, it is transferred to a water washing tank to remove acid and impurities.

[0024] S3 is crystallized, transferred to a crystallization tank for crystallization, and then the extracted oil is de-dried by a centrifuge to obtain a crude product.

[0025] S4 washing, separating the crude product through a centrifuge, dehydrating the extracted oil to obtain the crude product, putting the crude product into a washing kettle, adding detergent, stirring and washing;

[0026] S5 separation, using a fully automatic self-unloading centrifuge to separate the material from water to obtain a high-quality product, put it into a double-cone dryer for drying, and then pack the finished product.

[0027] First, take 50g of the reacted intermediate p...

Embodiment 2

[0033] S1 extraction, the materials reacted in the process of producing amantadine hydrochloride are extracted by extraction oil and then left to stand for stratification;

[0034] S2 is washed with water, and after the stratification is completed, it is transferred to a water washing tank to remove acid and impurities.

[0035] S3 is crystallized, transferred to a crystallization tank for crystallization, and then the extracted oil is de-dried by a centrifuge to obtain a crude product.

[0036] S4 washing, separating the crude product through a centrifuge, dehydrating the extracted oil to obtain the crude product, putting the crude product into a washing kettle, adding detergent, stirring and washing;

[0037] S5 separation, using a fully automatic self-unloading centrifuge to separate the material from water to obtain a high-quality product, put it into a double-cone dryer for drying, and then pack the finished product.

[0038] First, take 150g of the reacted intermediate ...

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PUM

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Abstract

The invention discloses a preparation method of high-purity amantadine hydrochloride. The method comprises the following steps: extraction: extracting the reacted material in the amantadine hydrochloride production process with extraction oil, and standing for layering; washing with water, layering, transferring into a washing kettle, and removing acid and impurities; crystallizing, transferring into a crystallization kettle, crystallizing, and drying the extract oil by a centrifuge to obtain a crude product; washing, separating the crude product by a centrifuge, drying the extract oil to obtain a crude product, putting the crude product into a washing kettle, adding a detergent, stirring and washing; and separating, separating the material from water by using a full-automatic self-discharging centrifuge to obtain a refined product, putting the refined product into a double-cone drying machine, drying, and packaging to obtain a finished product. In actual use, discharged wastewater isreduced, the water yield is low after the process is improved, the wastewater can be recycled in production, zero emission is achieved, and the purity of amantadine hydrochloride is improved to 99.96%from 99.15%; the maximum single impurity content is reduced from 0.26% to 0.03%; amantadine hydrochloride meets the requirements of most samples and reagents, and the recovery rate of amantadine hydrochloride is 89.5%.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing high-purity amantadine hydrochloride. Background technique [0002] Amantadine is the first antiviral drug approved in the United States. Davis first discovered its antiviral effect in 1964, and it was successively included in the British Pharmacopoeia, the US Pharmacopoeia, the Japanese Pharmacopoeia and the Chinese Pharmacopoeia. Domestic production began in 1971. Amantadine has antiviral properties and is administered orally for the treatment and prevention of influenza A and for the treatment of Parkinson's neurological disorders. It can also be used for the treatment of shingles and post-shingles neuralgia. At present, amantadine has been widely used in anti-influenza, and it is believed that administration of amantadine within 48 hours of onset can alleviate the symptoms of influenza A virus. Abroad, amantadine is used to prevent and treat influenza...

Claims

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Application Information

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IPC IPC(8): C07C211/38C07C209/84
CPCC07C209/84C07C2603/74C07C211/38
Inventor 刘晓黎刘涛邴亚芬杨渐飞孙倩
Owner 中涛新材料有限公司
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