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
  • Application Information

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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 indu

Method used

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  • Method for synthesizing and preparing amantadine dry product

Examples

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Example Embodiment

[0057]Example 1:

[0058]A method for synthesizing a synthesis of synthesis of sodium bromine, sodium blend, urea, sodium hydroxide, and hydrochloric acid, including sodium hydroxide, and hydrochloric acid, including the following steps:

[0059]A1: Synthesis of bromine diamonds;

[0060]A11: Preparation of raw materials, taking gold sodes: bromine: sodium bisulfite is 1: 2.2: 0.56;

[0061]A12: Grinding the diamond developed into a pre-dried flask, gradually adding liquid bromide under stirring, slow heating;

[0062]A13: After the reaction, the second day gradually heated to 45 degrees Celsius, drip 7% of sodium hydrogen sulfite;

[0063]A14: Filtration, filter cake washed to a pH of 7, naturally dried to give bromide diamonds;

[0064]A2: Hydrogenamine dry product by bromine diamondacity;

[0065]A21: Mix the bromine diatondic and urea in proportion 1: 0.45, and heat it heat;

[0066]A22: Naturally cooling, then excess concentrated hydrochloric acid, allowing it to add excess sodium hydroxide after suffici...

Example Embodiment

[0070]Example 2:

[0071]A method of preparing a synthesis of diamiacamine dry product, with a main synthetic feedstock comprising anacatene, nitric oxide, dichloromethane, ozone, sodium thiosulfate, ethanol - water and zinc, including the following steps:

[0072]B1: Synthesis of nitro compounds;

[0073]B11: The diamondane with dichloromethane is added to the flask in a proportion of 1 g: 120 mL, stirring at a certain temperature;

[0074]B12: 30 equivalents of nitrogen dioxide, in -70 to -80 degrees Celsius.

[0075]B13: At low speed to ozone, thirty minutes;

[0076]B14: The sodium hydrogencarbonate solution is then added, then the organic phase was washed to neutral.

[0077]B15: Turning after drying can be obtained from product 1-nitrate gold;

[0078]B2: Synthesis of diamine amine;

[0079]B21: Another flask, sequentially add ethanol-water mixed solution, ice acetic acid, zinc powder, and ammonium chloride, which is 25 ml: 0.5 mmol: 20 mmol: 0.3mmol, raised to reflux during agitation, and corrosion ;

[0...

Example Embodiment

[0090]Example 3:

[0091]A method for synthesizing a synthesis of diamiacamine, with a main raw material comprising anacaten, nitric oxide, ozone, hydrazine, ethanol, diethyl ether, 6-hydrogen chloride and activated carbon, comprising the steps of:

[0092]C1: Synthesis of nitro compound;

[0093]C11: The diamondane with dichloromethane was added to the flask in a ratio of 1 g: 120 mL, and stirred at a certain temperature;

[0094]C12: 30 equivalents of nitrogen dioxide in a certain condition.

[0095]C13: At low speed, ozone is available, and the reaction is 30 minutes;

[0096]C14: Sodium bicarbonate solution was then added, then washed the organic phase to neutral.

[0097]C15: Steam after drying can be obtained from 1-nitrogen-nitrate.

[0098]C2: Preparation of catalyst;

[0099]C21: Ethanol, diethyl ether and 6-hydrogen chloride were added to the flask according to 1 ml: 5 ml: 0.15 g of the scale;

[0100]C22: After using electromagnetic stirring, the 6-hydrolyvate solids were blown and added to the propor...

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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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