Continuous synthesis method for 2-methyl-5-nitroimidazole

A synthetic method, nitroimidazole technology, applied in the direction of organic chemistry, can solve the problems of poor market competitiveness, complex process route, long reaction time, etc., achieve high production efficiency, low reaction temperature, and suppress side reactions.

Inactive Publication Date: 2020-07-03
SHANDONG HIMILE CHEM TECH
View PDF0 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above three processes all belong to the batch method to produce 2-methyl-5-nitroimidazole, the process route is complicated, the reaction time is very long about 1-3h, the product yield is low, and the market competitiveness is poor
[0005] The nitrification reaction is a violent exothermic reaction, if it is not well controlled, it will cause flushing, and if it is serious, it will cause an explosion
Simultaneously, for the research of synthesizing 2-methyl-5-nitroimidazole in microreactor, there is no report at home and abroad

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A kind of continuous synthetic method of 2-methyl-5-nitroimidazole is as follows:

[0044] (1) Synthesis of 2-methylimidazole:

[0045] Hastelloy microreactor, 10 umbrella-shaped channels, channel size 1mm, total liquid holding capacity of microreactor 23.2mL, molar ratio of glyoxal to acetaldehyde is 1:1.2, ammonium bicarbonate and glyoxal and The acetaldehyde mixture is fed in a volume ratio of 7:30. Ammonium bicarbonate is heated and dissolved in water to be configured into 21.7% aqueous ammonium bicarbonate solution, and stored in a water bath at 20°C, the material is transported into the microchannel reactor at a speed of 3.5mL / min with a pump, and 40% ethyl alcohol The mixture of dialdehyde and 40% acetaldehyde is sent to the microchannel reactor at 15mL / min by another pump, and the temperature is controlled in sections. At 30°C, the residence time is 35s (the total residence time is 75s), and the cyclization reaction is carried out to obtain 2-methylimidazole. ...

Embodiment 2

[0051] A kind of continuous synthetic method of 2-methyl-5-nitroimidazole is as follows:

[0052] (1) Synthesis of 2-methylimidazole:

[0053] Hastelloy microreactor, 10 umbrella-shaped channels, channel size 1mm, total liquid holding capacity of microreactor 23.2mL, molar ratio of glyoxal to acetaldehyde is 1:1.2, ammonium bicarbonate and glyoxal and The acetaldehyde mixture is fed in a volume ratio of 7:30. Ammonium bicarbonate is heated and dissolved in water to form a 21.7% ammonium bicarbonate aqueous solution, and stored in a water bath at 20°C, the material is transported into the microchannel reactor at a speed of 7mL / min by a pump, and 40% ethylene dicarbonate The mixture of aldehyde and 40% acetaldehyde was transported to the microchannel reactor at 30mL / min by another pump, and the temperature was controlled in sections. The temperature of the four slices in the front section was controlled at 10°C, the residence time was 14s, and the temperature in the back sectio...

Embodiment 3

[0059] A kind of continuous synthetic method of 2-methyl-5-nitroimidazole is as follows:

[0060] (1) Synthesis of 2-methylimidazole:

[0061] Hastelloy microreactor, 10 umbrella-shaped channels, channel size 1mm, total liquid holding capacity of microreactor 23.2mL, molar ratio of glyoxal to acetaldehyde is 1:1.2, ammonium bicarbonate and glyoxal and The acetaldehyde mixture is fed in a volume ratio of 7:30. Ammonium bicarbonate is heated and dissolved in water to be configured into 21.7% aqueous ammonium bicarbonate solution, and stored in a water bath at 20°C, the material is transported into the microchannel reactor at a speed of 5.5mL / min with a pump, and 40% ethyl alcohol The mixture of dialdehyde and 40% acetaldehyde is delivered to the microchannel reactor at 23.5mL / min by another pump, and the temperature is controlled in sections. At 50°C, the residence time is 29s (the total residence time is 48s), and the cyclization reaction is carried out to obtain 2-methylimid...

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

PropertyMeasurementUnit
melting pointaaaaaaaaaa
Login to view more

Abstract

The invention provides a continuous synthesis method for 2-methyl-5-nitroimidazole. The 2-methyl-5-nitroimidazole is synthesized in a micro-channel reactor. The synthesis method provided by the invention can realize continuous synthesis, is safe and stable in production process, extremely short in reaction time and high in yield, and can reduce the usage amount of concentrated sulfuric acid and lower cost.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and relates to a continuous synthesis method of 2-methyl-5-nitroimidazole. Background technique [0002] 2-Methyl-5-nitroimidazole, English name 2-Methyl-5-ni-troimidazde, CAS No. 88054-22-2, molecular formula: C 4 h 5 N 3 o 2 , molecular weight 127.114, white or slightly yellow powder, hardly soluble in water, slightly soluble in methanol, soluble in dilute acid and dilute alkali, easy to oxidize and decompose at high temperature, melting point 252-254℃. [0003] 2-Methyl-5-nitroimidazole is a typical special fine chemical intermediate; (1) It can be used in the preparation of metronidazole. Metronidazole has a strong effect of killing trichomoniasis, and is the first choice drug for the treatment of vaginal trichomoniasis; it can be used to treat amoebic dysentery and amebic liver abscess, and its curative effect is similar to that of emetine; at the same time, metronidazole has an...

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): C07D233/92
CPCC07D233/92
Inventor 绳镇蔡文静肖淑焕王威张本松任苗苗
Owner SHANDONG HIMILE CHEM TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap