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

Method for preparing amide

An amide and ionic liquid technology, applied in the field of amide preparation, can solve the problems of equipment corrosion, low-value ammonium sulfate, environmental pollution, etc., and achieve the effect of not corroding pipeline equipment

Inactive Publication Date: 2013-04-17
CHINA PETROCHEM DEVMENT
View PDF2 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the conversion rate of cyclohexanone oxime in the whole reaction is almost 100%, and the selectivity of caprolactam is 99%, the whole reaction not only produces a large amount of low-value ammonium sulfate, but also the catalyzed concentrated sulfuric acid will cause corrosion and environmental pollution to the whole equipment. And other issues

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
  • Method for preparing amide
  • Method for preparing amide
  • Method for preparing amide

Examples

Experimental program
Comparison scheme
Effect test

Synthetic example 1-N

[0034] Synthesis example 1-N, the synthesis of the ionic liquid of N-dimethylaspartic acid sulfate

[0035] Take 25g of aspartic acid and place it in a 500ml round bottom bottle, add 60ml (concentration 37%) formaldehyde solution, then add 200ml water, and finally add 8g Pd / C. The air in the reaction bottle was replaced with hydrogen, and then the reaction bottle was placed in a hydrogen environment to react for 48 hours. After the reaction was completed, the residual hydrogen was replaced with nitrogen, and then heated to 90°C under reflux, and the Pd / C was filtered off at this high temperature to obtain a colorless aqueous solution. Concentrate the colorless aqueous solution, then azeotrope with 100ml toluene to further remove water, and finally dry the product in a high vacuum, then crush it with a spatula to obtain 28.92 g of N,N-Di Methylaspartic acid, yield: 95.54%.

[0036] Take 10g of dimethylaspartic acid and place it in a 250ml round bottom bottle, add 40ml of wate...

Synthetic example 2-N

[0037] The synthesis of the ionic liquid of synthetic example 2-N-methyl glutamic acid sulfate

[0038] Take 10g of glutamic acid and add it to a 250ml round bottom reaction bottle, then add 100ml of water and stir for 30 minutes, then take 20ml (concentration 37%) formaldehyde solution, add it to the reaction bottle, and place it at 80°C for reaction. After reacting for 3 hours, a yellow liquid was obtained. The liquid was concentrated, then azeotroped with 100 ml of toluene to further remove water, and finally the product was dried under vacuum to obtain 10.52 g of a yellow solid with a yield of 97.22%.

[0039] Add 100ml of water and 10.3g of the above-mentioned yellow solid (unsaturated intermediate) into the reaction flask), then add 5g of 10% Pd / C, replace the air in the reaction flask with hydrogen, carry out the reduction reaction under hydrogen, and carry out the reaction for 24 hours After the reaction is completed, replace the hydrogen with nitrogen, heat to 80°C, ...

Synthetic example 3-N

[0041] Synthesis of the ionic liquid of synthetic example 3-N-methylaspartic acid sulfate

[0042] Take 10g of aspartic acid and add it to a 250ml round-bottomed reaction flask, then add 100ml of water and stir for 30 minutes, then take 20ml (concentration 37%) formaldehyde solution, add it to the reaction flask, and place it at 80°C for reaction. After reacting for 3 hours, a yellow liquid was obtained. The yellow liquid was concentrated, then azeotroped with 100 ml of toluene to further remove water, and finally dried in vacuum to obtain 10.63 g of yellow solid with a yield of 97.52%.

[0043] 100ml of water and 10.5g of the above yellow solid were added to the reaction flask, and then 5g of 10% Pd / C was added to replace the air in the reaction flask with hydrogen, and the reaction flask was subjected to a reduction reaction under hydrogen for 24 hours. After the reaction was completed, the hydrogen was replaced with nitrogen, and then heated to 80° C., the Pd / C was filtere...

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 relates to a method for preparing amide, wherein an amino acid ionic liquid is used as a reaction medium and a catalyst for catalyzing the Beckmann rearrangement reaction of ketoxime to generate the amide. At mild reaction temperature and within ultrashort reaction time, the amino acid ionic liquid with an asymmetric characteristic is used for catalyzing the ketoxime to be rearranged to generate the amide without adding other catalysts, such as concentrated sulfuric acid. The method has the advantages of no pipeline equipment corrosion and high ketoxime conversion rate and amideselection rate.

Description

technical field [0001] The invention relates to a method for preparing amides, in particular to a method for preparing amides by using ionic liquids to catalyze ketoxime. Background technique [0002] In recent years, ionic liquids have been widely used in chemistry. From a practical point of view, ionic liquids refer to salt compounds with a melting point lower than 100°C. Ionic liquids are composed of anions and cations, with high polarity, low vapor pressure, low melting point, non-flammability, strong acid resistance, high temperature resistance, high conductivity, good electrochemical characteristics and wide liquid temperature range (-96 ° C to 400°C) and other special properties, it can be applied in many technologies such as chemical synthesis, catalytic reaction, electrochemistry, analytical chemistry and separation technology; because ionic liquid can be operated under normal pressure, it can replace the commonly used volatile organic solvent ( volatile organic c...

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): C07C231/10C07D201/04B01J31/04
Inventor 蔡东翰姚秉铎谢正发
Owner CHINA PETROCHEM DEVMENT
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