Process for high-yield preparation of amantadine hydrochloride

An amantadine hydrochloride, high-yield technology, applied in the field of high-yield preparation of amantadine hydrochloride, can solve the problems of difficulty in recovery, high price, strong corrosiveness, etc., achieves improved conversion rate and yield, and increased units Yield, the effect of improving yield

Inactive Publication Date: 2016-04-27
天津民祥生物医药股份有限公司
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Problems solved by technology

[0006] The raw materials used in the bromination route are usually prepared by excess bromine, which is not only expensive, but also highly corrosive and difficult to recycle, resulting in serious pollution

Method used

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  • Process for high-yield preparation of amantadine hydrochloride

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Experimental program
Comparison scheme
Effect test

Embodiment

[0047] A kind of high yield prepares the technique of amantadine hydrochloride, comprises the following steps:

[0048] (1) Preparation of 1-acetylaminoadamantane;

[0049] ① Prepare the raw materials;

[0050] ②Pre-cool the first reaction kettle with a specification of 50L in advance, gradually add 25L (47.5kg) of fuming sulfuric acid, stir for 10 minutes, and add 7.5kg of adamantane in batches at -5°C. Can not exceed 0 ℃, continue to stir for half an hour after adding;

[0051] ③At -5°C, add 6.5L (5.2kg) of acetonitrile dropwise. During the dropping process, the temperature should not exceed 0°C; keep stirring for half an hour after dropping, slowly raise the temperature to 35°C (room temperature), and keep the temperature for 3 hours;

[0052] ④ Slowly add 2.5kg of adamantane when the reaction solution becomes clear; keep the temperature from rising during the addition, and stir for another 3 hours after addition;

[0053] More was added and the temperature was raised to...

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Abstract

The invention discloses a process for high-yield preparation of amantadine hydrochloride; the process includes two steps of (1) preparation of 1-acetamidodamantane and (2) preparation of amantadine hydrochloride. Amantadine hydrochloride can be prepared in one reaction kettle, so the operation steps are simplified; in addition, by using a phase transfer catalyst, the reaction effect is promoted; with a selected solvent system after screening, the reaction conversion rate and yield are increased, and costs, energy consumption and environmental pollution are reduced.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a process for preparing amantadine hydrochloride with high yield. Background technique [0002] The common cold is one of the most common diseases that plague people, and it is also one of the most famous incurable diseases in the world. So far, humans cannot completely prevent the onset and infection of colds. Among various diseases, cold is the most common frequently-occurring disease. Correspondingly, the users of cold medicines are the most, and they constitute a huge cold medicine market. The cold medicine market is the most competitive field of OTC medicines in China. According to statistics, the total consumption of OTC medicines in China was about 30 billion yuan in 2003, and cold medicines accounted for nearly 15% of the total. The annual consumption was about 4 billion yuan, and the annual growth rate was over 20%. The attractive market space has attracted many pha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/62C07C211/38
CPCC07C209/62C07C231/06
Inventor 刘万里李彬曹晖李春贵于瑞林陈鑫
Owner 天津民祥生物医药股份有限公司
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