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Method for continuously synthesizing 1H-1,2,3-triazole by using microchannel reactor

A microchannel reactor, 1H-1 technology, applied in chemical instruments and methods, chemistry/physics/physicochemical reactors, organic chemistry, etc., can solve problems such as potential safety hazards

Active Publication Date: 2021-05-18
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to provide a kind of method that microchannel reactor continuously synthesizes 1H-1,2,3-triazole, selects the hydrogen peroxide of environmental protection for use As an oxidizing agent for oxidative ring formation, and then diazotized deamination reaction with nitrite, the entire reaction process is carried out in an aqueous solvent environment, without the need for replacement and addition of solvents, avoiding the use of toxic initial reactants, and No solid waste is generated, the use of microchannel reactors eliminates the amplification effect of two high reaction heats, and solves the problem of great safety hazards in the synthesis process of hydrogen peroxide oxidation and diazotization in traditional reactors, achieving green and safe

Method used

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  • Method for continuously synthesizing 1H-1,2,3-triazole by using microchannel reactor
  • Method for continuously synthesizing 1H-1,2,3-triazole by using microchannel reactor
  • Method for continuously synthesizing 1H-1,2,3-triazole by using microchannel reactor

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Experimental program
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Effect test

Embodiment 1

[0047]1) hydrazine hydrate aqueous solution (80%) 190g is delivered to preheating in the preheating module of microchannel reactor according to the flow rate of 40g / min, enters the first reaction module group of microchannel reactor after preheating, glyoxal Aqueous solution (40%) 200g is passed into the first reaction module by the flow velocity of 37.9g / min, and the first reaction module temperature is 100 ℃, and in the first reaction module, total residence time is 30s and hydrazine hydrate reacts, then in cooling The module was cooled to 30°C to obtain material 1;

[0048] 2) Material 1 continues to pass into the second reaction module, and at the same time, hydrogen peroxide solution (30%) is passed into the second reaction module at a flow rate of 32.6mL / min and undergoes oxidative cyclization reaction with material 1 at a reaction temperature of 30°C. The time is 30s, and the material 2 is obtained;

[0049] 3) Material 2 continues to pass into the third reaction modul...

Embodiment 2

[0053] 1) hydrazine hydrate aqueous solution (80%) 190g is delivered to preheating in the preheating module of microchannel reactor according to the flow rate of 40g / min, enters the first reaction module group of microchannel reactor after preheating, glyoxal Aqueous solution (40%) 200g is passed into the first reaction module by the flow rate of 40g / min, and the first reaction module temperature is 50 ℃, and in the first reaction module, total residence time is that 60s and hydrazine hydrate react, then in cooling module Cool down to 30°C to obtain material 1;

[0054] 2) Material 1 continues to pass into the second reaction module, and at the same time, hydrogen peroxide solution (30%) is passed into the second reaction module at a flow rate of 35mL / min to carry out oxidative cyclization reaction with material 1, the reaction temperature is 15°C, and the residence time Be 40s, make material 2;

[0055] 3) Material 2 continues to pass into the third reaction module of the mi...

Embodiment 3

[0059] 1) hydrazine hydrate aqueous solution (80%) 190g is delivered to preheating in the preheating module of microchannel reactor according to the flow rate of 40g / min, enters the first reaction module group of microchannel reactor after preheating, glyoxal Aqueous solution (40%) 200g passes into the first reaction module by the flow velocity of 35g / min, and the first reaction module temperature is 80 ℃, and in the first reaction module, total residence time is 42s and hydrazine hydrate reacts, then in cooling module Cool down to 35°C to obtain material 1;

[0060] 2) Material 1 continues to pass into the second reaction module, and at the same time, hydrogen peroxide solution (30%) is passed into the second reaction module at a flow rate of 39mL / min and undergoes oxidative cyclization reaction with material 1, the reaction temperature is 35 ° C, the residence time Be 30s, make material 2;

[0061] 3) material 2 continues to pass into the third reaction module of the microc...

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Abstract

The invention relates to a method for continuously synthesizing 1H-1,2,3-triazole through a microchannel reactor, and belongs to the technical field of medicine synthesis. The method comprises the following steps: reacting a hydrazine hydrate aqueous solution and a glyoxal aqueous solution in a micro-channel reactor to prepare a material 1, continuously reacting the material 1 with hydrogen peroxide in the micro-channel reactor to prepare a material 2, and continuously mixing the material 2 with concentrated hydrochloric acid in the micro-channel reactor to obtain a material 3; conducting reaction on the material 3 and a sodium nitrite aqueous solution in the micro-channel reactor, and conducting post-treatment to obtian 1H-1,2,3-triazole. No solvent needs to be added or replaced in the reaction process, manganese dioxide and potassium permanganate which can generate solid waste are prevented from being used, and toxic substances such as toluenesulfonyl chloride and dioxane which are harmful to the environment are not used either; and the 1H-1,2,3-triazole can be safely produced.

Description

technical field [0001] The invention relates to a method for continuously synthesizing 1H-1,2,3-triazole in a microchannel reactor, belonging to the technical field of pharmaceutical synthesis. Background technique [0002] 1H-1,2,3-triazole (C 2 h 3 N 3 ) is an important organic synthesis intermediate, which can be used to synthesize a variety of complex compounds in the fields of drugs, fungicides, etc., for example, it is one of the key intermediates in the synthesis of tazobactam. [0003] At present, the synthetic routes of 1H-1,2,3-triazole mainly include the following types: [0004] (1) Using o-phenylenediamine as a raw material, benzotriazole (2) is obtained through diazotization and ring closure reaction, and then oxidized by potassium permanganate to 1H-1,2,3-triazole- 4,5-dicarboxylic acid (3), and then catalyzed decarboxylation by copper powder in dioxane solvent to prepare 1H-1,2,3-triazole. [0005] [0006] This method uses dioxane as a solvent, the y...

Claims

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Application Information

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IPC IPC(8): C07D249/04C07C249/16C07C251/76B01J19/00
CPCC07D249/04C07C249/16C07C251/76B01J19/0093B01J2219/00867B01J2219/0254B01J2219/0263B01J2219/0286B01J2219/0295
Inventor 孙涛许鹤姜启英
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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