A kind of synthesis technique of 1h-1,2,4-triazole

Abstract

The invention discloses a synthesizing process of 1H-1,2,4-triazole, comprising the following synthesizing steps: (1) adding formic ether, hydrazine hydrate and ammonium salt in sequence into a high-pressure reaction kettle, pressurizing the reaction kettle and gradually heating up to a reaction temperature under a sealed stirring state, gradually lowering down the reaction temperature after the reaction is complete and using the after heat to evaporate the byproduct methyl alcohol, thereby obtaining a white emulsion matter; (2) transferring the white emulsion matter into the reaction kettle, adding ethyl alcohol, heating and refluxing to obtain a mixture solution, hot filtering the mixture solution by a filter cartridge into a crystallization kettle, cooling the filtrate inside the crystallization kettle to room temperature, separating out white crystals, drying by a hot air drying oven after centrifugal separation, thereby obtaining the 1H-1,2,4-triazole. The synthesizing process of the 1H-1,2,4-triazole allows the hydrazine hydrate to react with the formamide which is obtained by direct ammonolysis of the ammonia obtained from the decomposition of the formic ether and the ammonium salt under the high temperature conditions, thereby effectively increasing the entire chemical reaction speed, reducing the reaction temperature and increasing the product output, with simple overall synthesizing process, lower energy consumption and few three-waste discharge.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a synthesis process of 1H-1,2,4-triazole. Background technique [0002] The pure product of 1,2,4-triazole is white crystal, the industrial product is pink or brown solid, the melting point is 119°C-121°C, the decomposition temperature is above 220°C, it is easily soluble in water and slightly soluble in ethyl acetate , Acetone, insoluble in chloroform, benzene. [0003] Since J.A. Bladin synthesized 1,2,4-triazole for the first time in 1885, heterocyclic compounds containing 1,2,4-triazole have developed extremely rapidly. Chemical researchers all over the world have synthesized a large number of compounds containing 1,2,4-triazole, and found that such substances contain a variety of physiological activities, so after a hundred years of development, 1,2,4 - Triazoles are still valued by experts in drug synthesis, organic synthesis, and azole-containing materials all over the w...

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Problems solved by technology

[0009] (2) 1,3,5-triazine and hydrazine salt are mixed and refluxed in absolute ethanol to obtain 1,2,4-triazole, the synthetic process route is as follows, (relevant documents include Triazines.XVI.A new synthesis for 1,2,4-triazoles.Grundmann,Christoph and Ratz,Rudi.Journal of Organic Chemistry,1956.) This method is not suitable for large-scale industrial production due to the high cost of raw materials

Its reaction temperature and the speed of dehydration are the key conditions in the whole reaction process, so the relative energy consumption of the existing process as a whole is relatively high, and because of this, the process of 1H-1,2,4-triazole synthesis still needs further development optimization and improvement

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