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Method for preparing 5-methylpyrazine-2-carboxylic acid by catalytic oxidation

A methylpyrazine, catalytic oxidation technology, applied in chemical instruments and methods, heterogeneous catalyst chemical elements, physical/chemical process catalysts, etc., can solve the difficult synthesis and oxidation synthesis of 5-methyl porphyrin catalysts Pyrazine-2-carboxylic acid, high price and other problems, to achieve the effect of easy industrial scale production, easy control and low cost

Active Publication Date: 2019-02-22
LANZHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although this method is relatively green and environmentally friendly, the metalloporphyrin catalyst is difficult to synthesize and expensive, and it is not easy to be used in large-scale industrial catalytic oxidation to synthesize 5-methylpyrazine-2-carboxylic acid

Method used

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  • Method for preparing 5-methylpyrazine-2-carboxylic acid by catalytic oxidation

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Embodiment 1

[0024] A method for preparing 5-methylpyrazine-2-carboxylic acid by catalytic oxidation. At first, diatomite, manganese chloride, sodium tungstate, cobalt nitrate, and distilled water are added to the reactor according to the mass ratio of the following elements, silicon Alite: Mn: W: Co: H 2 O=1:0.03:0.03:0.05:50, stir magnetically at room temperature to disperse and absorb evenly, then remove water by evaporation, add liquid silica sol with 5% of the total mass of the solid sample and knead it into small particles of 1-2mm The samples were placed in a muffle furnace and calcined in an air atmosphere at 550°C for 5 hours to obtain Mn-W-Co / diatomaceous earth supported catalyst particles. Fill 10g of Mn-W-Co / diatomaceous earth catalyst particles into the fixed-bed microreactor reaction tube, raise the temperature of the reactor to 240°C, and use high-temperature steam to feed 2,5-dimethylpyrazine at 10ml / Introduce bubbling into the fixed bed reaction tube in 1 minute, and inj...

Embodiment 2

[0026] A method for preparing 5-methylpyrazine-2-carboxylic acid by catalytic oxidation. At first, diatomite, manganese chloride, sodium tungstate, cobalt nitrate, and distilled water are added to the reactor according to the mass ratio of the following elements, silicon Alite: Mn: W: Co: H 2 O=1:0.05:0.05:0.07:50, stir magnetically at room temperature to disperse and absorb evenly, then remove water by evaporation, add liquid silica sol with 5% of the total mass of the solid sample and knead it into small particles of 1-2mm The samples were placed in a muffle furnace and calcined in an air atmosphere at 600°C for 4 hours to obtain Mn-W-Co / diatomaceous earth supported catalyst particles. Fill 10g of Mn-W-Co / diatomite catalyst particles into the reaction tube of the fixed-bed microreactor, raise the temperature of the reactor to 300°C, and use high-temperature steam to feed 2,5-dimethylpyrazine at 10ml / Introduce bubbling into the fixed bed reaction tube in 1 minute, and injec...

Embodiment 3

[0028] A method for preparing 5-methylpyrazine-2-carboxylic acid by catalytic oxidation. At first, diatomite, manganese chloride, sodium tungstate, cobalt nitrate, and distilled water are added to the reactor according to the mass ratio of the following elements, silicon Alite: Mn: W: Co: H 2 O=1:0.07:0.06:0.09:50, stir magnetically at room temperature to disperse and absorb evenly, then remove water by evaporation, add liquid silica sol with 5% of the total mass of the solid sample and knead it into small particles of 1-2mm The samples were placed in a muffle furnace and calcined in an air atmosphere at 660°C for 5 hours to obtain Mn-W-Co / diatomaceous earth supported catalyst particles. Fill 10g of Mn-W-Co / diatomite catalyst particles into the fixed-bed microreactor reaction tube, raise the temperature of the reactor to 320°C, and use high-temperature steam to feed 2,5-dimethylpyrazine at 10ml / Introduce bubbling into the fixed bed reaction tube in 1 minute, and inject oxyge...

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Abstract

The invention discloses a method for preparing 5-methylpyrazine-2-carboxylic acid by catalytic oxidation. According to the invention, Mn-W-Co / diatomite is used as a catalyst, 2,5-dimethylpyrazine is used as a raw material, oxygen is used as an oxidant, and 5-methylpyrazine-2-carboxylic acid is synthesized by catalytic oxidation. The method comprises the following steps: packing Mn-W-Co / diatomite catalyst into a fixed bed reactor with temperature of 200-400 DEG C, introducing the reaction raw material 2,5-dimethylpyrazine into a reaction tube of the fixed bed reactor packed with Mn-W-Co / diatomite supported catalyst by bubbling with high temperature water vapor, introducing oxygen separately into the reaction tube, carrying out catalytic oxidation of 2,5-dimethylpyrazine in the catalyst bedto produce 5-methylpyrazine-2carboxylic acid, carrying the product out of the reaction tube by water vapor, condensing, crystallizing, and collecting. In the invention, the preparation method of the Mn-W-Co / diatomite catalyst is simple. The method for preparing 5-methylpyrazine-2carboxylic acid by continuous catalytic oxidation in the fixed bed is environmentally friendly, pollution-free, simple in operation, easy in control, high in 5-methylpyrazine-2-carboxylic acid yield and easy in industrial production.

Description

technical field [0001] The present invention relates to a kind of synthetic technology of important pharmaceutical intermediate 5-methylpyrazine-2-carboxylic acid, specifically a kind of 2,5-dimethylpyrazine is catalyzed and oxidized by a loaded catalyst to synthesize 5-methylpyrazine The method of pyrazine-2-carboxylic acid. technical background [0002] As an important pharmaceutical intermediate, 5-methylpyrazine-2-carboxylic acid is mainly used to synthesize hypoglycemic drug glipizide and blood pressure drug acipimox; at the same time, it can also be used to synthesize anti-tuberculosis drug 5 -Methylpyrazine-2-carboxylate. The large-scale synthesis of 5-methylpyrazine-2-carboxylic acid by an efficient, green, and environmentally friendly method is of great significance. At present, the industrial synthesis of 5-methylpyrazine-2-carboxylic acid uses 2,5-dimethylpyrazine as a raw material, and its synthetic route is shown in the following formula. The synthetic methods...

Claims

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Application Information

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IPC IPC(8): C07D241/24B01J23/889
CPCC07D241/24B01J23/002B01J23/8892B01J2523/00B01J2523/69B01J2523/72B01J2523/845Y02P20/584
Inventor 董正平
Owner LANZHOU UNIVERSITY
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