The synthetic method of triazole

A synthetic method, triazole technology, applied in the field of organic chemical synthesis, can solve the problems of no obvious advantages in comprehensive cost, difficult separation of formamide, high production cost, etc., and achieve low comprehensive cost, low equipment requirements, and few by-products Effect
CN104230830BInactive Publication Date: 2016-03-30重庆锦杉科技有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
重庆锦杉科技有限公司
Publication Date
2016-03-30
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention belongs to the technical field of organic chemical synthesis, particularly relates to a triazole synthesis method and aims at using methyl ethyl ketazine to replace hydrazine hydrate so as to provide a low-cost and high-yield 1,2,4-triazole preparation method. The technical scheme is that the triazole synthesis method comprises the following steps of enabling ammonia, hydrogen peroxide and butanone to react with the presence of formamide to prepare the methyl ethyl ketazine; separating an upper-layer oil phase containing the methyl ethyl ketazine from a water phase containing the formamide, evaporating the ammonia, the butanone and water in the water phase to recover the formamide; rising the temperature of the formamide to be 165 DEG C-190 DEG C, then dropwise adding the oil phase into the formamide, performing heat preservation reaction at the temperature ranging from 165 DEG C to 190 DEG C for 20-60 minutes, recovering incompletely-reacted methyl ethyl ketazine through distillation to obtain 1,2,4-triazole. By means of the triazole synthesis method, the 1,2,4-triazole with purity higher than 95% can be obtained, and the yield is higher than 95% (by formamide).
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Description

technical field

[0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a synthesis method of triazole. Background technique

[0002] 1,2,4-triazole is also known as 1H-1,2,4-triazole, TA-4 triazole brightener, 1,2,4-1H-triazole, triazole, etc., with With strong biological activity, it is widely used in organic synthesis fields such as pesticides, medicines, dyes and rubber additives, and is an important organic chemical intermediate. 1,2,4-Triazole and its derivatives have become one of the hot spots and key areas of drug research and development in recent years, and the market usage is increasing year by year.

[0003] At present, there are mainly four methods for synthesizing 1,2,4-triazoles:

[0004] (1) Formamide-hydrazine hydrate-ammonia gas method: This method is to react formamide and hydrazine hydrate to first synthesize bishydrazide, and then react with excess ammonia to form triazole. This method is divide...

Claims

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