High-yield amantadine preparation method

A high-yield technology for amantadine, applied in the field of high-yield amantadine preparation, can solve the problems of many by-products, waste of raw materials, low yield, etc., and achieve the effect of mild reaction and cost saving

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

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Problems solved by technology

[0004] The present invention solves the problems of many by-products in the prior art, waste of raw materials, low yield, high and violent reaction temperature, and provides a high-yield amantadine preparation method, which has mild reaction during

Method used

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  • High-yield amantadine preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0021] like figure 1 As shown, a method for preparing amantadine with high yield is as follows: condensation, bromination, urea and DMF are mixed and heated, and the solid is separated out and then kept warm; The solid was kept for 3 hours, and the mixed solution of water and DMF was continuously azeotropically distilled; distilled, an aqueous sodium hydroxide solution was prepared, added to the reactor in stages, and amantadine and water were azeotropically distilled; secondary crystallization, drying, Enter the plate and frame filter press to filter the finished product, and the yield of the finished product is 97.3%.

[0022] Specifically, in the S1 condensation step, after the materials are mixed and heated to 160-165°C, solids are precipitated, and the temperature is kept at 160-170°C for 1 hour;

[0023] Specifically, in the S2 dissolving step, the temperature is kept at 99-102° C. for 3 hours.

[0024] Specifically, the concentration of the sodium hydroxide aqueous so...

Embodiment 2

[0027] like figure 1 As shown, a method for preparing amantadine with high yield is as follows: condensation, bromination, urea and DMF are mixed and heated, and the solid is separated out and then kept warm; The solid was kept for 3 hours, and the mixed solution of water and DMF was continuously azeotropically distilled; distilled, an aqueous sodium hydroxide solution was prepared, added to the reactor in stages, and amantadine and water were azeotropically distilled; secondary crystallization, drying, Enter the plate and frame filter press to filter the finished product, and the yield of the finished product is 97.3%.

[0028] Specifically, in the S1 condensation step, after the materials are mixed and heated to 160-165°C, solids are precipitated, and the temperature is kept at 160-170°C for 1 hour;

[0029] Specifically, in the S2 dissolving step, the temperature is kept at 99-102° C. for 3 hours.

[0030] Specifically, the concentration of the sodium hydroxide aqueous so...

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PUM

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Abstract

The invention discloses a high-yield amantadine preparation method, which comprises the following steps: condensation: mixing bromo, urea and DMF, heating, separating out solids, and keeping the temperature; after dissolving and heat preservation are finished, washing off condensed solids, then carrying out heat preservation for 3 hours, and continuously carrying out azeotropic distillation to obtain water and a DMF mixed solution; distilling, preparing a sodium hydroxide aqueous solution, adding the sodium hydroxide aqueous solution into a reaction kettle by several times, and simultaneouslycarrying out azeotropic distillation to obtain amantadine and water; and carrying out secondary crystallization and drying, and carrying out filter pressing in a plate-and-frame filter press to obtainthe finished product with a yield of 97.3%. The process method is mild in reaction, so that all materials can fully react. The yield of amantadine is increased from about 87.10% to about 97.30%; byproducts are few, so that raw materials are saved, and the cost for treating and recycling the byproducts is reduced.

Description

technical field [0001] The invention relates to the field of extraction methods for organic compounds, in particular to a method for preparing amantadine with high yield. Background technique [0002] Amantadine is mainly used in the manufacture of an antiviral drug, amantadine hydrochloride, which is an intermediate product in the production process of the drug. The technological process of amantadine is as follows figure 1 As shown, the concrete production method is: after the reactor is heated to 170 ℃, bromadamantane and urea are added in the reactor, and the two undergo amination reaction to generate water-insoluble amantadine, because the reactant contains Water-insoluble impurities, the resulting amantadine and water-insoluble impurities are bound together to reduce the purity. In order to remove these water-insoluble impurities, after the reaction is completed, the amantadine is cooled to 100 ° C, and then added The drinking water separates the amantadine from the ...

Claims

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Application Information

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IPC IPC(8): C07C209/62C07C209/86C07C211/38
CPCC07C209/62C07C209/86C07C2603/74C07C211/38
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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