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Method for synthesizing and preparing amantadine dry product

A technology of amantadine dry product and amantadine, which is applied in the preparation of nitro compounds, amino compounds, organic compounds, etc., can solve the problem of raw material selection in the production process of proportional pollution, and achieve high conversion rate and equipment requirements The effect of simplicity and mild reaction process

Pending Publication Date: 2021-03-12
天津民祥药业有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] In the prior art, there are many methods for preparing amantadine in the laboratory state, but its proportion pollution, production process and raw material selection have not yet reached the standard of industrial production. How to ensure mild reaction, low pollution and comparatively high process steps Under easy conditions and can reach higher conversion rate, is the problem that the present invention aims to solve

Method used

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  • Method for synthesizing and preparing amantadine dry product

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Embodiment 1

[0058] A kind of amantadine dry product synthetic preparation method, its synthetic raw material comprises adamantane, bromine, sodium bisulfite, urea, sodium hydroxide and hydrochloric acid, comprises the steps:

[0059] A1: Synthesis of bromoadamantane;

[0060] A11: Raw material preparation, take adamantane: bromine: sodium bisulfite in a mass ratio of 1:2.2:0.56;

[0061] A12: Grind the adamantane and add it to the pre-dried flask, gradually drop into the liquid bromine under the condition of stirring, and heat slowly;

[0062] A13: Overnight after the reaction, gradually heat to 45 degrees Celsius the next day, and add dropwise a 7% solution prepared by sodium bisulfite;

[0063] A14: filter, wash the filter cake with water until the pH is 7, and dry naturally to obtain bromoadamantane;

[0064] A2: Synthesis of dry amantadine from bromoadamantane;

[0065] A21: Mix bromoadamantane and urea in a ratio of 1:0.45, and heat at a fixed temperature;

[0066] A22: Cool down...

Embodiment 2

[0071]A method for synthesizing and preparing amantadine dry product, its main synthetic raw materials include adamantane, nitrogen dioxide, methylene chloride, ozone, sodium thiosulfate, ethanol-water and zinc, comprising the following steps:

[0072] B1: Synthesis of nitro compounds;

[0073] B11: Add adamantane and dichloromethane into the flask according to the ratio of 1g:120ml, and stir at a certain temperature;

[0074] B12: Introduce 30 equivalents of nitrogen dioxide under the condition of -70 to -80 degrees Celsius,

[0075] B13: Introduce ozone at a low speed and react for 30 minutes;

[0076] B14: subsequent addition of sodium bicarbonate solution, subsequent washing of the organic phase to neutrality,

[0077] B15: The product 1-nitroadamantane can be obtained by rotary evaporation after drying;

[0078] B2: Synthesis of amantadine;

[0079] B21: Take another flask, add ethanol-water mixed solution, glacial acetic acid, zinc powder and ammonium chloride in seq...

Embodiment 3

[0091] A method for synthesizing and preparing dry amantadine, the main raw materials of which include adamantane, nitrogen dioxide, ozone, hydrazine hydrate, ethanol, ether, ferric chloride 6-hydrate and activated carbon, characterized in that it comprises the following steps:

[0092] C1: Synthesis of nitro compounds;

[0093] C11: Add adamantane and dichloromethane into the flask according to the ratio of 1g:120ml, and stir at a certain temperature;

[0094] C12: Introduce 30 equivalents of nitrogen dioxide under certain conditions,

[0095] C13: Introduce ozone at a low speed and react for 30 minutes;

[0096] C14: sodium bicarbonate solution is then added, the organic phase is then washed to neutrality,

[0097] C15: After drying, the product 1-nitroadamantane can be obtained by rotary evaporation;

[0098] C2: preparation of catalyst;

[0099] C21: Add ethanol, ether and ferric chloride 6-hydrate into the flask according to the ratio of 1ml: 5ml: 0.15g;

[0100] C22...

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Abstract

The invention discloses a synthesis and preparation method of an amantadine dry product, and relates to the technical field of amantadine preparation. The method mainly comprises adamantane, nitrogendioxide, ozone, hydrazine hydrate, ethanol, diethyl ether, ferric chloride hexahydrate and activated carbon, and comprises the following steps: synthesis of a nitro compound: adding adamantane and dichloromethane into a flask according to a ratio of 1g: 120ml, stirring at a certain temperature, introducing 30 equivalents of nitrogen dioxide under a certain condition, introducing ozone at a low speed, reacting for 30 minutes, adding a sodium bicarbonate solution, washing the organic phase to be neutral, performing drying, and carrying out rotary evaporation to obtain the product 1-nitro adamantane. The dry amantadine product is prepared through a hydrazine hydrate reduction method, corresponding purification is conducted, the whole reaction process is mild, the process steps are simple andconvenient, the requirement for equipment is simple, the conversion rate is very high, and the method has the value of industrial batch production popularization.

Description

technical field [0001] The invention relates to the technical field of amantadine synthesis, in particular to a synthesis and preparation method of amantadine dry product. Background technique [0002] Adamantane is a highly symmetrical cage-like hydrocarbon, and the entire ring system has the structural characteristics of positive symmetry and high stability, and under certain conditions, the adamantane molecule will also undergo skeleton rearrangement, oxidation, alkylation and other types of reactions Therefore, the adamantane molecule has strong designability, so it has a wide range of uses in medicine, functional polymers, lubricants, surfactants, catalysts, photographic materials, etc., and is called a new generation of fine chemical raw materials. [0003] In the prior art, there are many methods for preparing amantadine in the laboratory state, but its proportion pollution, production process and raw material selection have not yet reached the standard of industrial ...

Claims

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Application Information

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IPC IPC(8): C07C209/34C07C211/38C07C209/84
CPCC07C209/325C07C201/08C07C209/84C07C2603/74C07C211/38C07C205/05
Inventor 李彬刘万里李春贵许晓勇
Owner 天津民祥药业有限公司
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