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

Synthesis method of 2-methyl-5-vinylpyridine

A technology of vinylpyridine and synthesis method, applied in the direction of organic chemistry, etc., can solve the problems of large amount of chemical raw materials, complex synthesis process, unfriendly environment, etc., achieve wide application value, simplify the treatment process, and reduce the effect of experimental steps

Active Publication Date: 2017-01-25
西安天一生物技术股份有限公司
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the current 2-methyl-5-vinylpyridine synthesis method, there are complex synthesis techniques, high cost, low yield, large amount of chemical raw materials, and unfriendly defects to the environment

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
  • Synthesis method of 2-methyl-5-vinylpyridine
  • Synthesis method of 2-methyl-5-vinylpyridine
  • Synthesis method of 2-methyl-5-vinylpyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) Take 350ml of metal-organic reducing reagent and place it in a 1000ml four-necked bottle, cool down to -10°C, dissolve 65 grams of 6-methylnicotinic acid methyl ester in 200ml of ether organic solvent and slowly add it dropwise into the four-necked bottle , the dropping time should not be less than 2h, and the whole system should replace the air with nitrogen before dropping;

[0037] 2) Put 173g of methyl bromide triphenylphosphonium salt into a 2L four-necked bottle, add 400ml of ether organic solvent, when the temperature of the solvent in the bottle drops below 5°C, add 57g of potassium tert-butoxide in batches, and wait until the reaction is over Continue to stir for 1h and set aside;

[0038]3) Slowly add the reaction solution obtained in 1) to 2), and control the rate of addition. During the reaction, the temperature of the reaction solution will rise, and the temperature should not exceed 10°C. After the addition is completed, continue the reaction for 30 min...

Embodiment 2

[0040] The inventive method comprises:

[0041] 1) At a temperature of -10 to 15°C, dissolve methyl 6-methylnicotinate in an ether organic solvent to obtain solution A, slowly add solution A to the metal organic reducing reagent, and add solution A dropwise The time to the metal organic reducing reagent is not less than 2h, and the reaction environment during the dropwise addition adopts a nitrogen atmosphere to obtain solution B; the ether organic solvent is diethyl ether, and the metal organic reducing reagent is organometallic lithium, 6-methyl nicotinic acid The ratio of the quality of the methyl ester to the volume of the ether organic solvent is 1:3, the ratio of the quality of 6-methyl nicotinic acid methyl ester to the volume of the metal organic reducing agent is 1:1;

[0042] 2) Take methyl bromide triphenylphosphonium salt and add ether organic solvent to obtain solution C, add potassium tert-butoxide to solution C at a temperature below 5°C for reaction, stir after...

Embodiment 3

[0045] The inventive method comprises:

[0046] 1) At a temperature of -10 to 15°C, dissolve methyl 6-methylnicotinate in an ether organic solvent to obtain solution A, slowly add solution A to the metal organic reducing reagent, and add solution A dropwise The time to the metal organic reducing reagent is not less than 2h, and the reaction environment during the dropwise addition adopts a nitrogen atmosphere to obtain solution B; the ether organic solvent is methyl tert-butyl ether, and the metal organic reducing reagent is organometallic lithium and organic Metal copper, the ratio of the quality of 6-methyl nicotinic acid methyl ester and the volume of ether organic solvent is 1:4, the ratio of the quality of 6-methyl nicotinic acid methyl ester and the volume of metal organic reducing reagent is 1 :1.2;

[0047] 2) Take methyl bromide triphenylphosphonium salt and add ether organic solvent to obtain solution C, add potassium tert-butoxide to solution C at a temperature bel...

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 discloses a synthesis method of 2-methyl-5-vinylpyridine. The synthesis method aims at reducing synthetic steps, simplifying processing procedures, increasing yield, saving costs, reducing the use of chemical raw materials and protecting the environment effectively. The technical scheme adopted is: (1) reducing the raw material methyl 6-methylnicotinate to 2-methyl-5-pyridyl formaldehyde; (2) preparing a phosphorus ylide reagent; and (3) reacting 2-methyl-5-pyridyl formaldehyde with the phosphorus ylide reagent to prepare 2-methyl-5-vinylpyridine, and conducting concentrated rectification to prepare the product.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis of pharmaceutical intermediates and novel materials, and in particular relates to a synthesis method of 2-methyl-5-vinylpyridine. Background technique [0002] 2-Methyl-5-vinylpyridine has a wide application value in the research and development of new organic materials and new drugs, and is an important monomer. For example, it can be copolymerized with butadiene and styrene emulsion to obtain butadiene pyridine latex for dipping cords; adding polyacrylonitrile can improve its dyeing power. And can be polymerized into excellent cation exchange resin. In the current 2-methyl-5-vinylpyridine synthesis method, there are disadvantages such as complex synthesis process, high cost, low yield, large amount of chemical raw materials, and unfriendly to the environment. Contents of the invention [0003] In order to solve the problems in the prior art, the present invention proposes a 2- Syn...

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
IPC IPC(8): C07D213/127C07D213/16C07D213/48
CPCC07D213/127C07D213/16C07D213/48
Inventor 姚卫帮王霄
Owner 西安天一生物技术股份有限公司
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

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com