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Method for preparing pyrazinamide

A technology of pyrazinamide and methylpyrazine, which is applied in the field of preparing pyrazinamide, can solve the problems of affecting product quality and product yield, difficulty in controlling pyrazinic acid, and high production cost, and achieves low cost, simple operation, The effect of high yield

Inactive Publication Date: 2017-08-04
SUZHOU HOMESUN PHARMA
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Problems solved by technology

[0004] The main by-product of 2-cyanopyrazine is pyrazinic acid during hydrolysis, and the preparation of pyrazinamide is basically realized by the method of heating acid-base catalysis in the existing reported literature, but there are few synthetic techniques in the existing reports. It is difficult to control the production of pyrazinic acid, the main impurity in the reaction, which affects the quality and yield of the product. The preparation process still needs to be refined to achieve a product that meets the quality standard, which will cause excessive production costs.

Method used

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  • Method for preparing pyrazinamide
  • Method for preparing pyrazinamide
  • Method for preparing pyrazinamide

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 300L of purified water and 20kg of 2-methylpyrazine to a 500L reactor, control the temperature of the reaction system at 3-5°C, and continuously inject ammonia until the pH of the reaction system reaches 12 to 12.5. The pH of the reaction system will follow the reaction. However, by intermittently supplementing ammonia, the pH of the system is controlled to stabilize between 12 and 12.5. After about 2 hours of reaction, the raw material disappears, and the content of pyrazinic acid is 0.15%. It is directly filtered and dried to obtain 25.5kg of pyrazinamide. Rate: 98.4%, purity> 99.9%.

Embodiment 2

[0022] Add 800L of purified water and 80kg of 2-methylpyrazine to a 1000L reactor, control the temperature of the reaction system at 5-8°C, and continuously inject ammonia until the pH of the reaction system reaches 12-12.3. The pH of the reaction system will follow the reaction. However, by intermittently supplementing ammonia gas, the pH of the system was controlled to stabilize between 12 and 12.3. After about 1 hour of reaction, the raw materials disappeared, and the content of pyrazinic acid was 0.12%. It was directly filtered and dried to obtain 102kg of pyrazinamide. The yield : 97.5%, purity> 99.9%.

Embodiment 3

[0024] Add 600L of purified water and 30kg of 2-methylpyrazine to a 1000L reactor, control the temperature of the reaction system at 3-6°C, and continuously inject ammonia until the pH of the reaction system reaches 12.2-12.5. The pH of the reaction system will follow the reaction. However, by intermittently supplementing ammonia gas, the pH of the system was controlled to stabilize between 12.2-12.5. After about 3 hours of reaction, the raw materials disappeared, and the content of pyrazinic acid was 0.1%. The pyrazinamide was directly filtered and dried to obtain 38.8kg of pyrazinamide. Rate: 98.9%, purity> 99.9%.

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Abstract

The invention discloses a method for preparing pyrazinamide. The method is characterized by comprising the following steps: controlling the temperature of a reaction system at 3-6 DEG C, introducing ammonia gas into a 2-methylpyrazine water solution in a mass ratio of (1 to 10)-(1 to 20), and maintaining the pH at 12-12.5; and reacting for 1-4 hours, and carrying out throw filtration and drying, so as to obtain pyrazinamide. The method provided by the invention is simple and convenient in operation, high in yield and quality and low in cost.

Description

Technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing pyrazinamide. Background technique [0002] Pyrazinamide is an important anti-tuberculosis drug. It is mainly used for chronic tuberculosis, fever, cough, and sputum. The minimum inhibitory concentration (MIC) is 20mg / L. It has an inhibitory effect on the tubercle bacillus in the cell, and can enter the cell and enter the brain tissue through the blood-brain barrier to kill the tuberculosis bacillus; it has a unique sterilization effect on the semi-dormant bacteria that slowly metabolizes in the macrophages, so it is tuberculosis One of the main drugs for short-term chemotherapy. [0003] At present, the domestic synthetic route of pyrazinamide mainly adopts 2-cyanopyrazine as the raw material to prepare by hydrolysis, and mainly adopts acid-base catalysis or biocatalysis. Due to the high cost of biocatalysis, most of the domestic ones still use acid-base cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/24
CPCC07D241/24
Inventor 樊超翟金星陆志丹
Owner SUZHOU HOMESUN PHARMA
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