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Amantadine hydrochloride impurity removal method

A technology for amantadine hydrochloride and amantadine, which is applied in the preparation of amino compounds from amines, purification/separation of amino compounds, and organic chemistry, etc. Synthesis process, cost reduction effect

Pending Publication Date: 2021-03-12
天津民祥药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of amantadine hydrochloride in the above-mentioned patent has the following disadvantages: using oleum, a large amount of acid waste gas will be generated in the reaction process, a large amount of water needs to be added for dilution in the post-treatment process, and the amount of waste water is serious

Method used

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  • Amantadine hydrochloride impurity removal method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A method for removing impurities of amantadine hydrochloride, such as figure 1 shown, including the following steps:

[0037] S1: Take 15g of refined amantadine bromide and 10g of urea, stir, mix and grind, and pass through a 200-mesh sieve;

[0038] S2: Move the mixture to a 100ml three-necked bottle, and add 40ml of soybean oil;

[0039] S3: Heat the temperature of the oil bath to 140°C, put it into a three-neck bottle, continue heating to 160°C, keep it warm, react to 190°C, stop the heating when the reaction is over;

[0040] S4: Keep the temperature of the oil bath at 160°C for 15 minutes, transfer to a beaker after cooling to room temperature;

[0041] S5: Add 115ml of 2mol / L hydrogen chloride into the beaker, heat to dissolve, cool to 50°C after dissolving, filter, boil the filter cake with 45ml of mol / L hydrogen chloride for 20min, cool to 50°C, filter twice, and combine twice the filtrate;

[0042] S6: Put the filtrate into a separatory funnel and let it st...

Embodiment 2

[0058] A method for removing impurities of amantadine hydrochloride, such as figure 1 shown, including the following steps:

[0059] S1: Take 15g of refined amantadine bromide and 10g of urea, stir, mix and grind, and pass through a 200-mesh sieve;

[0060] S2: Move the mixture to a 100ml three-necked bottle, and add 40ml of soybean oil;

[0061] S3: Heat the temperature of the oil bath to 140°C, put it into a three-neck bottle, continue heating to 160°C, keep it warm, react to 190°C, stop the heating when the reaction is over;

[0062] S4: Keep the temperature of the oil bath at 160°C for 15 minutes, transfer to a beaker after cooling to room temperature;

[0063] S5: Add 115ml of 2mol / L hydrogen chloride to the beaker, heat to dissolve, cool to 50°C after dissolving, filter, boil the filter cake with 45ml of mol / L hydrogen chloride for 20min, cool to 50°C, filter twice, and combine twice the filtrate;

[0064] S6: Put the filtrate into a separatory funnel and let it stan...

Embodiment 3

[0079] A method for removing impurities of amantadine hydrochloride, such as figure 1 shown, including the following steps:

[0080] S1: Take 15g of refined amantadine bromide and 10g of urea, stir, mix and grind, and pass through a 200-mesh sieve;

[0081] S2: Move the mixture to a 100ml three-necked bottle, and add 40ml of soybean oil;

[0082] S3: Heat the temperature of the oil bath to 140°C, put it into a three-neck bottle, continue heating to 160°C, keep it warm, react to 190°C, stop the heating when the reaction is over;

[0083] S4: Keep the temperature of the oil bath at 160°C for 15 minutes, transfer to a beaker after cooling to room temperature;

[0084] S5: Add 115ml of 2mol / L hydrogen chloride to the beaker, heat to dissolve, cool to 50°C after dissolving, filter, boil the filter cake with 45ml of mol / L hydrogen chloride for 20min, cool to 50°C, filter twice, and combine twice the filtrate;

[0085] S6: Put the filtrate into a separatory funnel and let it stan...

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Abstract

The invention discloses an amantadine hydrochloride impurity removal method, and relates to the technical field of chemical synthesis. The problem that waste gas and waste water are generated by usingfuming sulfuric acid is solved. The preparation method specifically comprises the following steps: taking 15g of refined bromo-amantadine and 10g of urea, stirring, mixing and grinding, and sieving with a 200-mesh sieve; transferring the mixture into a 100ml three-necked bottle, and adding 40ml of soybean oil; heating the oil bath to 140 DEG C, putting the oil bath into a three-neck bottle, continuously heating to 160 DEG C, keeping the temperature, reacting to 190 DEG C, and stopping heating after the reaction is finished. Brominated amantadine and urea are used as raw materials, soybean oilis used as a solvent, the reaction temperature is controlled to be 160 DEG C, the synthesis process of amantadine hydrochloride is improved, an impurity-removed pure amantadine hydrochloride productis obtained through hydrolysis, decoloration and purification, generation of waste gas is effectively reduced, and the problem of environmental pollution in the amantadine hydrochloride synthesis process is solved; compared with the prior art, wastewater is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for removing impurities of amantadine hydrochloride. Background technique [0002] Domestic amantadine raw materials are mainly used in compound anti-cold preparations, accounting for about 77% of the total. Due to incomplete statistics on supply and export, the actual export volume is about 30 tons. The output of amantadine single preparations is relatively stable, and the annual consumption of amantadine is relatively stable. About 10 tons of raw materials. The amantadine veterinary drug market is growing year by year. The traditional preparation of amantadine adopts the route of first bromination and then ammonification, or first nitration and then reduction. The raw materials used in the bromination route are usually prepared by excess bromine, which is not only expensive , is also highly corrosive and difficult to recycle, resulting in serious pollution....

Claims

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Application Information

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IPC IPC(8): C07C209/84C07C209/68C07C211/38
CPCC07C209/84C07C209/68C07C2603/74C07C211/38
Inventor 刘万里李彬李春贵陈瑞香
Owner 天津民祥药业有限公司
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