Synthesizing technology of triazole derivative

Abstract

The invention belongs to the field of medicine processing, and specifically relates to a synthesizing technology of a triazole derivative. The synthesizing technology provided by the invention is advantaged in that: the raw materials are easy to obtain, the time consumption is low, the condition is mild, and the yield is high. A technical scheme adopted by the invention comprises steps that: methanamide is added into a four-port flask provided with a stirrer, a constant-temperature dropping funnel, a distillation apparatus and a tail gas absorbing apparatus; methanamide is heated to a temperature of 175-190 DEG C; hydrazine hydrate is dropped into methanamide, wherein a molar ratio of methanamide to hydrazine hydrate is 1:1.1-1:2; the dropping is finished in 0.5-2.5h; emitted ammonia gas is delivered into an absorbing bottle to be absorbed, wherein the absorbing bottle contains 20-30% H2SO4; when dropping is finished, the temperature is maintained for 0.5-2.5h; the materials are cooled; when a large amount of crystals are precipitated, the materials are subject to pump filtration, such that a crude product is obtained; the crude product is washed by using ethyl acetate, such that a target product 1H-1,2,4-triazole is obtained. A yield is calculated, and a melting point is detected.

Description

technical field [0001] The invention belongs to the field of medicine processing, and more specifically relates to a synthesis technique of triazole derivatives. Background technique [0002] 1H-1,2,4-triazole is an important medicine, pesticide and dye intermediate. Especially in the field of medicine, triazole pharmacophore has lower toxicity than imidazole and exhibits various biological activities, such as antifungal, antibacterial, antituberculosis, antiviral, etc. 1H-1,2,4-triazole and its derivatives have become one of the hotspots and focuses of drug research and development in recent years. [0003] At present, there are four main methods for synthesizing 1H-1,2,4-triazole: [0004] (1) Prepared by the reaction of formamide and formamide. The raw materials of this method are relatively expensive, and most of them use excess formamide as a solvent. After-treatment, formamide needs to be evaporated under reduced pressure. The operation is very complicated. If it is ...

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Problems solved by technology

[0004] (1) Prepared by the reaction of formamide and formamide. The raw materials of this method are relatively expensive, and most of them use excess formamide as a solvent. After-treatment, formamide needs to be evaporated under reduced pressure. The operation is very complicated. If it is not handled properly, the yield will be greatly reduced. Rate;

[0005] (2) It is prepared from three raw materials of formic acid, hydrazine hydrate, and formamide. This method uses more raw materials, and the double-tube feeding method has strict requirements on the feeding speed, and the reaction is divided into two stages. The process is more complicated and the production cycle is longer;

[0006] (3) Feed ammonia gas into formic acid earlier to generate ammonium formate, then add hydrazine hydrate dropwise. The first step of this method is to feed ammonia gas into a two-phase reaction, the reaction conditions are harsh, the reaction time is long, and the operation is more complicated;

[0007] (4) Prepared from formamide and hydrazine hydrate, this method is simple and convenient, the yield is high, the reaction time is 4.5-5h, and it needs to stand overnight to wait for crystallization, and the production cycle is long

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