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

A kind of synthetic method of 3,5-dimethyl-4-nitropyridine-n-oxide

A technology of lutidine and nitropyridine, which is applied in the field of synthesis of 3,5-dimethyl-4-nitropyridine-N-oxide, and can solve problems such as bad operating environment, serious problems, and equipment corrosion , to achieve the effect of friendly operating environment, short reaction time and reducing environmental pressure

Active Publication Date: 2017-01-04
JIANGSU ZHONGBANG PHARMA
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But no matter which one it is, a lot of brownish-yellow smoke will be produced during the reaction and post-processing, not only the operating environment is not good, but also the equipment is corroded more seriously.

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
  • A kind of synthetic method of 3,5-dimethyl-4-nitropyridine-n-oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 12.3g of 3,5-lutidine-N-oxide in 90g of concentrated sulfuric acid, add dropwise a sulfuric acid solution of potassium nitrate (potassium nitrate 14.15g, concentrated sulfuric acid 100g ). After the dropwise addition was completed, the reaction was carried out at a temperature of 60° C. to 65° C. for 2 hours. HPLC monitoring until complete reaction of starting material. Cool down to room temperature, add water and stir, adjust pH to 8-8.5 with ammonia water, filter and dry to obtain 14.4 g of light yellow 3,5-dimethyl-4-nitropyridine-N-oxide, HPLC purity 99%, yield The rate is 85.7%.

Embodiment 2

[0025] Dissolve 12.3g of 3,5-lutidine-N-oxide in 188g of concentrated sulfuric acid, add dropwise a sulfuric acid solution of potassium nitrate (40.44g of potassium nitrate, 600g of concentrated sulfuric acid) at a temperature of 20°C to 30°C ). After the dropwise addition was completed, the reaction was carried out at a temperature of 110° C. to 120° C. for 0.5 hours. HPLC monitoring until complete reaction of starting material. Cool down to room temperature, add water and stir, adjust the pH to 8-8.5 with ammonia water, filter, and dry to obtain 14.5 g of light yellow 3,5-dimethyl-4-nitropyridine-N-oxide, HPLC purity 99%. The yield is 86.3%.

Embodiment 3

[0027] Dissolve 12.3g of 3,5-lutidine-N-oxide in 65g of concentrated sulfuric acid, and dropwise add sulfuric acid solution of potassium nitrate (potassium nitrate 10.11g, concentrated sulfuric acid 60g) at a temperature of 10°C to 15°C ). After the dropwise addition is completed, the reaction is carried out at a temperature of 85° C. to 90° C. for 1 hour. HPLC monitoring until complete reaction of starting material. Cool down to room temperature, add water and stir, adjust pH to 8-8.5 with ammonia water, filter and dry to obtain 14.3 g of light yellow 3,5-dimethyl-4-nitropyridine-N-oxide, HPLC purity 99%, yield rate of 85%.

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 3,5-dimethyl-4-nitropyridine-N-oxide, which belongs to the field of chemical industry. The method is to mix 3,5-lutidine-N-oxide and concentrated sulfuric acid to form a mixed solution, and add the sulfuric acid solution of potassium nitrate dropwise to the mixed solution at a temperature of 0°C to 60°C , and then react at a temperature of 60°C to 120°C for 0.5 to 12 hours to prepare 3,5-dimethyl-4-nitropyridine-N-oxide. The synthetic method of 3,5-dimethyl-4-nitropyridine-N-oxide of the present invention adopts potassium nitrate as a nitrating reagent, instead of concentrated nitric acid or fuming nitric acid, the reaction time is greatly shortened, and during the reaction and aftertreatment process There is also no brownish-yellow smoke, and the operation environment is friendly, reducing the environmental pollution caused by the large use of nitric acid, and the reaction yield has also increased. Today, environmental issues are getting more and more attention, and it can be a good substitute for nitric acid as nitrification The reagent completes the nitration reaction.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a synthesis method of 3,5-dimethyl-4-nitropyridine-N-oxide. Background technique [0002] 3,5-Dimethyl-4-nitropyridine-N-oxide is an important pharmaceutical intermediate, which can be used to synthesize omeprazole and esomeprazole. Use 3,5-lutidine as the starting material, add hydrogen peroxide and a suitable catalyst to obtain 3,5-lutidine-N-oxide, then add concentrated nitric acid / sulfuric acid or fuming nitric acid / sulfuric acid as a mixed acid The nitrating reagent can be used to produce 3,5-dimethyl-4-nitropyridine-N-oxide. [0003] Concentrated sulfuric acid plays a catalytic and dehydrating role in the nitration reaction. When the concentrated nitric acid of 65%~68% is adopted as the nitrating reagent, due to the high water content in the concentrated nitric acid, the reaction is affected in the presence of water, resulting in a decrease in the yield and a ...

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 Patents(China)
IPC IPC(8): C07D213/89
CPCC07D213/89
Inventor 邢光才李维思徐强薛谊陈国萍赵光荣
Owner JIANGSU ZHONGBANG PHARMA
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