Method for preparing 3-diethylamino-n,n-diethylpropionamide by amidation, catalyst and application thereof

A technology based on diethylpropionamide and diethylamine, which is applied in the direction of carboxylic acid amide preparation, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc., which can solve the problem of large catalyst consumption and reaction temperature Advanced problems, to achieve the effect of stable product performance, lower reaction temperature and high catalytic efficiency

Active Publication Date: 2021-11-09
山东瑞博龙化工科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2012, Lundberg et al. used titanium tetrachloride and zirconium tetrachloride to catalyze the formylation reaction of phenylacetic acid and amine, and the conversion rate was as high as 99%, but the reaction temperature was high (120°C) and the amount of catalyst was large , is 20% of the substrate (see literature 2)

Method used

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  • Method for preparing 3-diethylamino-n,n-diethylpropionamide by amidation, catalyst and application thereof
  • Method for preparing 3-diethylamino-n,n-diethylpropionamide by amidation, catalyst and application thereof
  • Method for preparing 3-diethylamino-n,n-diethylpropionamide by amidation, catalyst and application thereof

Examples

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Embodiment 1

[0052] A method for preparing 3-diethylamino-N,N-diethylpropionamide by amidation, comprising the steps of:

[0053] (1) Measure 4.5g of multi-walled carbon nanotubes (length is 10-20nm, specific surface area is 523m 2 / g, internal diameter is 5-8nm, and external diameter is 12-16nm), pours in the three-necked flask that has condensing tube, adds the concentrated sulfuric acid that 9.0g mass concentration is 12.6% and the concentrated nitric acid that 2.25g mass concentration is 22.3% The mixed solution was heated to 40°C for ultrasonic dispersion for 1h with a power of 200W. After completion, it was washed 7 times with distilled water, and then vacuum-dried at -0.098Mpa and 80°C for 12h to obtain oxidized multi-walled carbon nanotubes.

[0054] (2) The oxidized multi-walled carbon nanotubes are transferred to a three-necked flask connected with a condenser tube, a vacuum pump, and a separatory funnel placed in an oil bath heating. In the separatory funnel, the mass concentrat...

Embodiment 2

[0058] A method for preparing 3-diethylamino-N,N-diethylpropionamide by amidation, comprising the steps of:

[0059] (1) Measure 4.5g of multi-walled carbon nanotubes (length is 10-20nm, specific surface area is 523m 2 / g, internal diameter is 5-8nm, and external diameter is 12-16nm), pours in the three-necked flask that has condenser, adds the concentrated sulfuric acid that 10.8g mass concentration is 12.6% and the concentrated nitric acid that 2.7g mass concentration is 22.3% The mixed solution was heated to 45°C for ultrasonic dispersion for 1.2h with a power of 300w, washed 5 times with distilled water, and then vacuum-dried at -0.098Mpa and 70°C for 14h to obtain oxidized multi-walled carbon nanotubes.

[0060] (2) Transfer the oxidized multi-walled carbon nanotubes to a three-necked flask connected with a condenser, a vacuum pump, and a separatory funnel placed in an oil bath heating. In the separatory funnel, the concentration after dehydration and deoxidation of 12.0 ...

Embodiment 3

[0064] A method for preparing 3-diethylamino-N,N-diethylpropionamide by amidation, comprising the steps of:

[0065] (1) Measure 4.5g of multi-walled carbon nanotubes (length is 10-20nm, specific surface area is 523m 2 / g, internal diameter is 5-8nm, external diameter is 12-16nm), pours in the three-necked flask that has condensing tube, adds the concentrated sulfuric acid that 9.6g mass concentration is 12.6% and the concentrated nitric acid that 2.4g mass concentration is 22.3% The mixed solution was heated to 50°C for ultrasonic dispersion for 1.5h with a power of 500w, washed with distilled water for 6 times, and then vacuum-dried at -0.098Mpa and 90°C for 16h to obtain oxidized multi-walled carbon nanotubes.

[0066] (2) The dried multi-walled carbon nanotubes are transferred to a three-necked flask connected with a condenser tube, a vacuum pump, and a separatory funnel placed in an oil bath heating. In the separatory funnel, the concentration after dehydration and deoxid...

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Abstract

The present invention relates to the technical field of 3-diethylamino-N, N-diethylpropionamide, in particular to a method for preparing 3-diethylamino-N, N-diethylpropionamide by amidation and its catalyst and application . The method is as follows: after mixing 3-diethylaminopropionate methyl ester, carbon nanotube-loaded 2-amino-5-naphthol-7-sulfonic acid catalyst and organic titanium catalyst promoter, stir evenly, and then add dried Diethylamine reacts under heating conditions, that is, too. The method of the present invention adopts carbon nanotube-supported 2-amino-5-naphthol-7-sulfonic acid compounded with an organic titanium catalyst promoter, and has the advantages of less catalyst consumption, high catalytic efficiency, stable product performance, and high conversion rate (up to 92% or more) and other advantages; and the reaction process only needs to be carried out at 90-95°C under normal pressure. Compared with the existing method that needs to be carried out under high temperature and high pressure, the method of the present invention has obvious technical advantages.

Description

technical field [0001] The present invention relates to the technical field of 3-diethylamino-N,N-diethylpropionamide, in particular to a method for preparing 3-diethylamino-N,N-diethylpropionamide by amidation and its catalyst and application . Background technique [0002] The information disclosed in the Background of the Invention is only intended to increase the understanding of the general background of the invention, and is not necessarily to be taken as an acknowledgment or any form of suggestion that the information constitutes the prior art that is already known to those skilled in the art. [0003] 3-Diethylamino-N,N-diethylpropionamide is an important amide compound. Its pyrolysis products are stable, non-toxic, odorless, non-corrosive, and can be miscible with water or most organic solvents. In the fields of UV ink, 3D printing, cosmetics, photoresist, etc., it plays an important role in "industrial yeast" and "industrial monosodium glutamate". "The role. [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10C07C231/02C07C237/06
CPCB01J31/2295B01J35/1004B01J2531/0225B01J2531/46C07C231/02C07C237/06
Inventor 郑万强姚慧玲国凤玲耿超群谢呈鹏王红乐
Owner 山东瑞博龙化工科技股份有限公司
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