Preparation process of pyrazinamide

A technology of pyrazinamide and its preparation process, which is applied in the field of pyrazinamide preparation process, can solve the problems of no specific description of the synthetic route, short synthesis steps and overall yield, and achieve the advantages of production cost control, increase of total yield, Effects with a wide range of applications

Inactive Publication Date: 2020-07-14
SUZHOU HOMESUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The Chinese patent application number is CN201310454127.6, which discloses a small molecule inhibitor of plant ethylene synthesis pathway, pyrazinamide, which is a specific inhibitor of ACC oxidase (ACO), and can inhibit the ethylene synthesis precursor ACC in the plant ethylene synthesis pathway. Converted to ethylene, the synthetic route is not specified, and the technical effect of shorter synthetic steps and higher overall yield is not achieved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Synthesis of 2-Methylpyrazine

[0040] (1) Reaction: Put catalyst 1 in reactor 1, pass in nitrogen gas, check the airtightness of the reaction pipeline, and discharge the air in reactor 1 at the same time, the flow rate of nitrogen gas is 0.2L / min, heat the reactor 1. Control the temperature rise rate, and finally rise to 360°C; during the temperature rise period, while maintaining the total gas flow at 0.2L / min, slowly increase the ratio of hydrogen and nitrogen until they are finally equal, and the catalyst 1 is reduced for 4 hours; the B2 Amine and 1,2-propanediol are mixed in an equimolar ratio and enter a preheater at 300°C through a metering pump. After reactor one is heated to a predetermined temperature, it enters reactor one for a gas-solid phase contact catalytic reaction. The mixture enters the receiver after being cooled by the condenser, and the exhaust gas is taken after being absorbed and then emptied and separated to obtain the 2-methylpyrazine;

[0041...

Embodiment 2

[0057] Synthesis of 2-Methylpyrazine

[0058] (1) Reaction: Put catalyst 1 in reactor 1, pass in nitrogen gas, check the airtightness of the reaction pipeline, and discharge the air in reactor 1 at the same time, the flow rate of nitrogen gas is 0.2L / min, heat the reactor 1. Control the temperature rise rate, and finally rise to 360°C; during the temperature rise period, while maintaining the total gas flow at 0.2L / min, slowly increase the ratio of hydrogen and nitrogen until they are finally equal, and the catalyst 1 is reduced for 4 hours; the B2 Amine and 1,2-propanediol are mixed in an equimolar ratio and enter a preheater at 300°C through a metering pump. After reactor one is heated to a predetermined temperature, it enters reactor one for a gas-solid phase contact catalytic reaction. The mixture enters the receiver after being cooled by the condenser, and the exhaust gas is taken after being absorbed and then emptied and separated to obtain the 2-methylpyrazine;

[0059...

Embodiment 3

[0075] Synthesis of 2-Methylpyrazine

[0076] (1) Reaction: Put catalyst 1 in reactor 1, pass in nitrogen gas, check the airtightness of the reaction pipeline, and discharge the air in reactor 1 at the same time, the flow rate of nitrogen gas is 0.2L / min, heat the reactor 1. Control the temperature rise rate, and finally rise to 360°C; during the temperature rise period, while maintaining the total gas flow at 0.2L / min, slowly increase the ratio of hydrogen and nitrogen until they are finally equal, and the catalyst 1 is reduced for 4 hours; the B2 Amine and 1,2-propanediol are mixed in an equimolar ratio and enter a preheater at 300°C through a metering pump. After reactor one is heated to a predetermined temperature, it enters reactor one for a gas-solid phase contact catalytic reaction. After the mixture is cooled by the condenser, it enters the receiver, and the exhaust gas is taken after being absorbed, emptied, and separated to obtain the 2-methylpyrazine;

[0077] (2) ...

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Abstract

A preparation process of pyrazinamide comprises the following steps: (1) synthesis of 2-methylpyrazine: putting a catalyst I into a reactor I, and performing reducing for 4 hours; adding 2-methylpyrazine into the reactor I, then adding ethylenediamine and 1, 2-propylene glycol, carrying out gas-solid phase contact catalytic reaction in the reactor I, cooling a mixture generated by the reaction through a condenser, feeding the mixture into a receiver, taking tail gas, and performing absorbing, emptying and separating to obtain 2-methylpyrazine, (2) chemical base catalysis; putting the catalystII into a reactor II, introducing an aqueous solution of 2-methylpyrazine in a mass ratio of (1:10)-(1:20) into the reactor II through a metering pump, introducing ammonia gas and air, controlling thetemperature of the reaction system to be 3-6 DEG C, maintaining the pH value to be 9-10, performing reacting for 1-2 hours, and performing heating to 20-30 DEG C to obtain 2-cyanopyrazine; and (3) synthesis of pyrazinamide. The preparation process of pyrazinamide has the advantages of the simple process, the high conversion rate, no generation of by-product pyrazinic acid, the good economic benefits and the wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of drug synthesis, and in particular relates to a preparation process of pyrazinamide. Background technique [0002] Pyrazinamide, molecular formula C 5 h 5 N 3 O, relative molecular weight 123.12, pKa0.5, sublimation begins at 159°C, melting point 189°C-191°C, boiling point 210°C-215°C. White crystalline powder, slightly bitter taste, odorless, soluble in water, slightly soluble in ethanol, chloroform, hardly soluble in ether. The aqueous solution is neutral and stable at room temperature. [0003] Pyrazinamide is an important first-line anti-tuberculosis drug. Its antibacterial mechanism is the same as that of p-aminosalicylic acid (PAS). PAS, puromycin strong, but less than isoniazid and streptomycin. When pyrazinamide is used alone, Mycobacterium tuberculosis rapidly develops resistance to it, but it has a synergistic effect when used in combination with rifampicin and isoniazid. In addition to be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D241/24
CPCC07D241/24
Inventor 樊超陆红彬
Owner SUZHOU HOMESUN PHARMA
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