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Method for preparing high purity 1H-1,2,3-triazole

A 1H-1 and triazole technology, applied in the field of high-purity 1H-1, can solve the problems of low purity of the final product, dangerous process operation, and large amount of waste water, so as to improve the shelf life, improve product quality, and reduce waste water The effect of production volume

Active Publication Date: 2010-05-26
LANXI SUNHOW FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above synthetic routes have problems such as large amount of waste water, dangerous and difficult process operation, low purity of final product (up to 98%) or short storage period.

Method used

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  • Method for preparing high purity 1H-1,2,3-triazole
  • Method for preparing high purity 1H-1,2,3-triazole
  • Method for preparing high purity 1H-1,2,3-triazole

Examples

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Embodiment 1

[0036] 1. In a 1000ml four-necked bottle, add 750ml of water, then add 120g of benzotriazole, raise the temperature to 60°C~70°C, and then slowly add 360g of potassium permanganate above 60°C. After the addition of potassium manganate, keep it warm at 60°C-100°C for 2 hours, filter while it is hot, concentrate the filtrate to about 300ml, cool to room temperature, adjust the solution to pH=2 with concentrated hydrochloric acid, stir for half an hour, and filter with a small amount of The filter cake was washed with water and dried at 80°C to 90°C for 4 hours. Add the dried filter cake to 3 times the amount of methanol, reflux and stir for half an hour, cool to room temperature, filter with suction, and dry at 80°C to 90°C for 3 hours to obtain 1H-1,2,3-triazole- 122g of 4,5-dicarboxylic acid, melting point 199°C-201°C, yield 77.7%.

[0037] 2. Add 122g of 1H-1,2,3-triazole-4,5-dicarboxylic acid obtained in the previous step into a 500ml three-necked flask, then add a catalyti...

Embodiment 2

[0040] 1. In a 1000ml four-necked bottle, add 750ml of water, then add 120g of benzotriazole, raise the temperature to 60°C~70°C, and then slowly add 360g of potassium permanganate above 60°C. After adding potassium manganate, keep it warm at 60°C-100°C for 2 hours, filter while hot, concentrate the filtrate to about 300ml, cool to room temperature, adjust the solution to pH=2 with 40% sulfuric acid solution, stir for half an hour, and pump Filter, wash the filter cake with a small amount of water, and dry at 80°C to 90°C for 4 hours. Add the dried filter cake to 4 times the amount of ethanol, reflux and stir for half an hour, cool to room temperature, filter with suction, and dry at 80°C to 90°C for 3 hours to obtain 1H-1,2,3-triazole- 113 g of 4,5-dicarboxylic acid, melting point 200°C-202°C, yield 71.9%.

[0041] 2. Add 113g of 1H-1,2,3-triazole-4,5-dicarboxylic acid obtained in the previous step into a 500ml three-necked flask, then add a catalytic amount of copper powder...

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Abstract

Disclosed is a preparation method to obtain a high purity 1H-1, 2, 3-triazole, in the process of which benzotriazole and potassium permanganate serve as raw materials. The raw materials are oxidized to open rings and acided to get 1H-1, 2, 3-triazole-4, 5-dicarboxylic acid crude product, which is to be refined by strong polar solvents. The refined 1H-1, 2, 3-triazole-4, 5-dicarboxylic acid turns into the raw oil of 1H-1, 2, 3-triazole after going through vacuum decarboxylation at the temperature of 100 -180 DEG C and with the help of catalysts. Under the action of lewis acid, the raw oil is finally converted into high purity 1H-1, 2, 3-triazole product whose purity reaches 99.5 per cent through oxidation, decoloration by activated carbon, and distillation. Nitrogen gas or inert gas is usedto interchange air in the wrapping barrel during the process of package so that the objectives of sound quality and long duration are achieved.

Description

technical field [0001] The invention relates to a preparation method of high-purity 1H-1,2,3-triazole, which belongs to the technical field of fine chemical preparation. Background technique [0002] 1H-1,2,3-Triazole has a structure as shown in Formula 1, and is an important intermediate for the synthesis of the novel β-lactamase inhibitor tazobactam. In addition, high-purity 1H-1,2 , 3-triazole is also used in cleaning agents for electronic products. [0003] [0004] Formula 1 [0005] The preparation method of high-purity 1H-1, 2, 3-triazole mainly contains at present bibliographical reports: directly use azide acid and acetylene to react under high temperature and high pressure and make; Take glyoxal as raw material, in butyl acetate and Prepared by rearrangement in the presence of toluene (see patent CN1242996); prepared by using p-toluenesulfonyl chloride and hydrazine hydrate as raw materials, and cyclized with glyoxal ("China Pharmaceutical Industry Journal" 20...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/04
Inventor 李惠跃姜维斌童小兵
Owner LANXI SUNHOW FINE CHEM