Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Process for synthesizing triazole derivative

A technology of triazole derivatives and synthesis process, applied in the direction of organic chemistry, etc., can solve the problems of harsh reaction conditions, long production cycle, complicated process, etc., and achieve the effects of mild reaction conditions and short time-consuming

Inactive Publication Date: 2013-04-03
李兰心
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Process for synthesizing triazole derivative
  • Process for synthesizing triazole derivative
  • Process for synthesizing triazole derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0016] The process steps of the present invention are: adding formamide into a four-necked flask equipped with a stirrer, a constant pressure dropping funnel, a distillation device and an exhaust gas absorption device, heating to 175-190°C, adding dropwise hydrazine hydrate, 1 / 3 formamide The molar ratio of amide to hydrazine hydrate is 1:1.1 to 1:2, after 0.5 to 2.5 hours of dripping, introduce the escaped ammonia gas into the absorption bottle (containing 20%-30%H 2 SO 4 ) absorption; after the dropwise addition, keep warm for 0.5-2.5h; cool, and after a large amount of crystals are precipitated, filter with suction to obtain a crude product, wash with ethyl acetate to obtain the target product 1H-1,2,4-triazole, and calculate the product rate, measuring melting point.

[0017] The reaction equation is:

[0018]

[0019] The present invention selects the mol ratio of 1 / 3 formamide and hydrazine hydrate, reaction temperature, dripping time, soaking time as 1H-1,2, the in...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the field of medicament processing and particularly relates to a process for synthesizing a triazole derivative. The process has the advantages that the raw materials are easily available, time consumption is low, reaction conditions are mild and yield is high. According to the technical scheme, the process comprises the following steps: adding formamide to a four-necked flask which contains a stirrer, a constant-pressure dropping funnel, a distillation device and a tail-gas absorption device; heating to a temperature of 175-190 DEG C; dropwise adding hydrazine hydrate for 0.5-2.5 hours, wherein the molar ratio of formamide to hydrazine hydrate is 1:(1.1-2); introducing the escaping ammonia into an absorption bottle filled with 20-30% H2SO4; preserving heat for 0.5-2.5 hours after finishing adding dropwise; cooling and filtering after a large amount of crystals are separated, to obtain a crude product; washing the crude product by ethyl acetate to obtain the target product which is 1H-1,2,4-triazol; calculating the yield; and measuring the melting point.

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 hot spots 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 ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/08
Inventor 李兰心
Owner 李兰心
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products