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Novel technology for preparing 1-acetamidodamantane

A technology of acetamido gold and adamantane, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, organic chemistry, etc., can solve the problems of high price, difficulty in recycling, strong corrosion, etc., and increase the unit output and increase the feeding rate Ratio, the effect of increasing the yield

Inactive Publication Date: 2016-02-24
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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  • Novel technology for preparing 1-acetamidodamantane

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Embodiment

[0029] A new process for preparing 1-acetylaminoadamantane, comprising the following steps:

[0030] ① Prepare the raw materials;

[0031] 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;

[0032] 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;

[0033] 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;

[0034] More was added and the temperature was raised to 20°C. Stir for half an hour. Let stand for about half an hour. Separa...

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Abstract

The invention discloses a novel technology for preparing 1-acetamidodamantane. Oleum which is environment-friendly, low in harm to human bodies and simple to control and adopts the looser control standard is used for replacing a halogen (bromine) used in the traditional technology; other raw materials mainly include adamantane, acetonitrile, dichloromethane and alkaline water; compared with the traditional technology for preparing 1-acetamidodamantane, the technology can increase the yield; particularly, the adamantane is added in batches, about 1 / 4 of the adamantane is added after the temperature gets close to the room temperature, the reaction progress can be better controlled, acid and the acetonitrile can be utilized to the maximum extent, the ingredient proportion of the adamantane is increased, and the yield per unit is increased.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a new process for preparing 1-acetylaminoadamantane. 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 pharmaceutical c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/58C07C231/06
CPCC07C231/06
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