Eureka AIR delivers breakthrough ideas for toughest innovation challenges, trusted by R&D personnel around the world.

Preparation method of N-pyridine oxide

A technology for oxidizing pyridine and pyridine, which is applied in the field of preparation of pyridine N-oxide, can solve the problems of long stable operation period and low conversion rate of pyridine, and achieve good catalytic effect, high yield and high atom utilization

Active Publication Date: 2011-05-18
SHANGHAI TIANYANG HOT MELT ADHESIVE CO LTD +1
View PDF4 Cites 12 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN101570509 proposes a method for preparing pyridine N-oxide. In this method, pyridine, oxygen, hydrogen, diluent gas, solvent and catalyst are mixed and contacted for reaction. The catalyst used is a microporous titanium silicon material or contains the microporous The composition of titanium silicon materials, the method has good selectivity and long stable operation period, but the conversion rate of pyridine is still low

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

[0014] 2.5g Na 2 WO 4 2H 2 O was dissolved in 30 mL of deionized water at 70°C, stirred and dissolved, and then 0.26 g of H with a mass fraction of 86% was added dropwise. 3 PO 4 , and then add 0.28 g mass fraction of 3% H 2 o 2 . Continue to stir the reaction until the solution is clear; after cooling down to room temperature, weigh 24.25g of silicon dioxide and add it to the above solution, stir well and let it stand for 20h, then evaporate the surface moisture at 105°C. After the above solid was dried at 115°C for 24h, it was placed in a muffle furnace and calcined at 300°C for 4h to obtain 26.07g of phosphorus-tungsten-silicon composite catalyst. Add 100g of pyridine and 26.07g of catalyst into a three-necked flask with a reflux condenser, a separatory funnel and an electric stirrer, and add 215g of 30% H 2 o 2 , H 2 o 2 Add dropwise within 30min, wait for H 2 o 2 After the dropwise addition was completed, the reaction was incubated at 80° C. for 120 minutes. ...

Embodiment 2

[0016] 5g Na 2 WO 4 2H 2 O was dissolved in 25 mL of deionized water at 70°C, stirred and dissolved, and then 0.64 g of H with a mass fraction of 86% was added dropwise. 3 PO 4 , and then add 0.5 g of 3% H 2 o 2 . Continue to stir the reaction until the solution is clear; after cooling down to room temperature, weigh 20.63g of silicon dioxide and add it to the above solution, stir well and let it stand for 20h, then evaporate the surface moisture at 105°C. After the above solid was dried at 115°C for 24h, it was placed in a muffle furnace and calcined at 300°C for 4h to obtain 24.27g of phosphorus-tungsten-silicon composite catalyst. Add 162g of pyridine and 24.27g of catalyst into a three-necked flask with a reflux condenser, a separatory funnel and an electric stirrer, and add 418g of 30% H 2 o 2 , H 2 o 2 Add dropwise within 30min, wait for H 2 o 2 After the dropwise addition was completed, the reaction was incubated at 65° C. for 50 minutes. Pour the mixture a...

Embodiment 3

[0018] 10g Na 2 WO 4 2H 2 O was dissolved in 40 mL of deionized water at 70°C, stirred and dissolved, and 1.38 g of H with a mass fraction of 86% was added dropwise. 3 PO 4 , and then add 2.0 g of 3% H 2 o 2 . Continue to stir the reaction until the solution is clear; after cooling down to room temperature, weigh 16g of silicon dioxide and add it to the above solution, stir well and let stand for 20h, then evaporate the surface moisture at 105°C. After the above solid was dried at 115°C for 24h, it was placed in a muffle furnace and calcined at 300°C for 4h to obtain 23.28g of phosphorus-tungsten-silicon composite catalyst. Add 100g of pyridine and 23.28g of catalyst into a three-necked flask with a reflux condenser, a separatory funnel and an electric stirrer, and add 240g of 30% H 2 o 2 , H 2 o 2 Add dropwise within 30min, wait for H 2 o 2 After the dropwise addition was completed, the reaction was incubated at 80° C. for 70 minutes. Pour the mixture after the r...

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 preparation method of N-pyridine oxide. The preparation method is characterized by comprising the following steps of preparing a phosphorus-tungsten-silicon composite catalyst by taking sodium tungstate, phosphoric acid and silicon dioxide as raw materials, and oxidizing pyridine under the action of the catalyst by taking hydrogen peroxide solution as an oxidizer to obtain the target product. The invention solves the problems of long reaction time, large energy consumption, complex post-treatment and the like in the traditional preparation method of the N-pyridine oxide, and optimizes the technological line of the reaction. The preparation method has the advantages of simple process, mild reaction condition and fast reaction speed, is convenient to operate, and is suitable for industrial production; in addition, the transformation ratio of the pyridine is high.

Description

technical field [0001] The invention relates to a preparation method of pyridine N-oxide, in particular to a preparation method of pyridine N-oxide based on a phosphorus-tungsten-silicon composite catalyst. Background technique [0002] Pyridine N-oxide is an important pharmaceutical and pesticide intermediate. For example, in medicine, it is an important intermediate for the synthesis of 2-chloromethyl-4-methoxy-3,5-lutidine hydrochloride, and it is also an important intermediate for the preparation of cardiotonic agents, bactericides, antiarrhythmic drugs, and An important intermediate of ulcer medicine, etc. According to different reaction mechanisms, the preparation of pyridine N-oxide can be divided into peroxide oxidation and catalytic oxidation. Hydrogen peroxide, benzoic acid peroxide, peracetic acid, phthalic acid peroxide, etc. are often used as oxidizing agents. The peroxide oxidation method has the advantages of simple process, mild conditions, cheap raw mater...

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): C07D213/89B01J27/188
Inventor 曾作祥张攀李哲龙朱万育孔庆娟韩涛
Owner SHANGHAI TIANYANG HOT MELT ADHESIVE CO LTD
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
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