阅读说明：本技术 2-甲基-1,2,4-***-3-胺的合成方法 (Synthesis method of 2-methyl-1, 2, 4-triazole-3-amine ) 是由 张大为 周强 高明飞 姚宝元 兰倩倩 赵廷 王曦 卫维 魏昕睿 谭汝鹏 贾涛 于 2020-05-20 设计创作，主要内容包括：本发明涉及一种2-甲基-1,2,4-三唑-3-胺的合成方法,主要解决目前没有适合工业化合成方法的技术问题。本发明分三步,第一步,首先由化合物1在溶剂1,4-二氧六环中加入N,N-二甲基甲酰胺二甲基缩醛反应得到化合物2,第二步,化合物2与三苯基膦,偶氮二羧酸二异丙酯在甲醇中反应得到化合物3,第三步,化合物3与氢氧化钠在甲醇和水中反应得到最终化合物4,反应式如下：<Image he="99" wi="551" file="100004_DEST_PATH_IMAGE002.GIF" imgContent="drawing" imgFormat="GIF" orientation="portrait" inline="no"></Image>。(The invention relates to a synthetic method of 2-methyl-1, 2, 4-triazole-3-amine, which mainly solves the technical problem that no industrial synthetic method is available at present. The invention comprises three steps, wherein in the first step, a compound 1 is added with N, N-dimethylformamide dimethyl acetal in a solvent 1, 4-dioxane to react to obtain a compound 2, in the second step, the compound 2 reacts with triphenylphosphine and diisopropyl azodicarboxylate in methanol to obtain a compound 3, and in the third step, the compound 3 reacts with sodium hydroxide in methanol and water to obtain a final compound 4, wherein the reaction formula is as follows: 。)

1. A synthetic method of 2-methyl-1, 2, 4-triazole-3-amine is characterized by comprising the following steps: the method comprises the following steps of firstly, adding N, N-dimethylformamide dimethyl acetal into a 1, 4-dioxane solvent from a compound 1 to react to obtain a compound 2, secondly, reacting the compound 2 with triphenylphosphine and diisopropyl azodicarboxylate in methanol to obtain a compound 3, and thirdly, reacting the compound 3 with sodium hydroxide in methanol and water to obtain a final compound 4, wherein the reaction formula is as follows:

。

2. the process for synthesizing 2-methyl-1, 2, 4-triazol-3-amine according to claim 1, wherein: the reaction temperature in the first step is 100 ℃, and the reaction time is 5 hours.

3. The process for synthesizing 2-methyl-1, 2, 4-triazol-3-amine according to claim 1, wherein: the second step reaction temperature is 25 ℃, and the reaction time is 12 hours.

4. The process for synthesizing 2-methyl-1, 2, 4-triazol-3-amine according to claim 1, wherein: the third step is carried out at 70 ℃ overnight.

Technical Field

The invention relates to a synthetic method of a compound 2-methyl-1, 2, 4-triazole-3-amine.

Background

The compound 2-methyl-1, 2, 4-triazole-3-amine (CAS: 15795-39-8) and related derivatives have wide application in medicinal chemistry and organic synthesis. At present, the synthesis method of 2-methyl-1, 2, 4-triazole-3-amine is only reported in documents. Therefore, it is necessary to develop a synthesis method which has easily available raw materials, convenient operation, easy control of reaction, proper overall yield and suitability for industrial production.

Disclosure of Invention

The invention aims to develop a synthetic method of 2-methyl-1, 2, 4-triazole-3-amine, which has the advantages of easily obtained raw materials, convenient operation, easily controlled reaction and higher yield. Mainly solves the technical problem that no industrial synthesis method is available at present.

The technical scheme of the invention is as follows: the invention relates to a method for synthesizing 2-methyl-1, 2, 4-triazole-3-amine, which comprises three steps, wherein in the first step, compound 1 is added with N, N-dimethylformamide dimethyl acetal in solvent 1, 4-dioxane for reaction to obtain compound 2, in the second step, compound 2 is reacted with triphenylphosphine and diisopropyl azodicarboxylate in methanol to obtain compound 3, and in the third step, compound 3 is reacted with sodium hydroxide in methanol and water to obtain final compound 4. The reaction formula is as follows:

the first step is at 100 deg.C for 5 hours; the second step is that the reaction temperature is 25 ℃ and the reaction time is 12 hours; the third step is carried out at 70 ℃ overnight.

The Chinese explanation of the invention is as follows: TLC: thin layer chromatography.

The invention has the beneficial effects that: the reaction process of the invention has reasonable design, adopts the raw material 3-amino-1, 2, 4-triazole which is easy to obtain and can be produced in large scale, and synthesizes the 2-methyl-1, 2, 4-triazole-3-amine through three steps, the method has short route, the yield can reach 40.5 percent, the reaction is easy to amplify, and the operation is convenient.

Detailed Description

The reaction formula of the invention is as follows: