A kind of synthetic method of n,n-dimethylamino ethyl acrylate

A technology for the synthesis of ethyl dimethylaminoacrylate, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as harsh process conditions, unsuitable for industrial production, and high by-products, and achieve friendly reaction conditions , Low production cost and reduced by-products

Active Publication Date: 2021-11-16
ZHEJIANG BENLI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the problems of harsh process conditions, high by-products, low yield, high cost and unsuitability for industrial production in the prior art.

Method used

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  • A kind of synthetic method of n,n-dimethylamino ethyl acrylate
  • A kind of synthetic method of n,n-dimethylamino ethyl acrylate
  • A kind of synthetic method of n,n-dimethylamino ethyl acrylate

Examples

Experimental program
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Effect test

Embodiment 1

[0066] Add ethyl acetate (88g, 1mol), dimethylamine (45g, 1mol), xylene 250mL and solid base catalyst 4.4g into the autoclave, feed CO, control the pressure to 1MPa and raise the temperature to 50°C, keep stirring and react for 4h , the CO pressure no longer drops, cool to room temperature, filter, reclaim the solid base catalyst, divide the water layer after adding the solvent xylene to the filtrate, reclaim the solvent (xylene) in the organic layer, and distill the residue under reduced pressure; collect 118~121°C ( 7.5mmHg) to obtain 136.3g of N,N-ethyl dimethylaminoacrylate as the target product, with a yield of 95.3% and an HPLC content of 99.8%.

Embodiment 2

[0068] Add ethyl acetate (88g, 1mol), dimethylamine (54g, 1.2mol), xylene 250mL and solid base catalyst 4.4g into the autoclave, feed in CO, control the pressure to 1MPa and raise the temperature to 50°C to keep stirring and react 4h, the pressure of CO no longer drops, cool to room temperature, filter, recover the solid base catalyst, add the solvent xylene to the filtrate and separate the water layer, recover the solvent (xylene) from the organic layer, and distill the residue under reduced pressure; collect 118~121 °C (7.5 mmHg) fraction, 136.5 g of the target product N,N-ethyl dimethylaminoacrylate was obtained, the yield was 95.5%, and the HPLC content was 99.5%.

Embodiment 3

[0070] Add ethyl acetate (88g, 1mol), dimethylamine (45g, 1mol), xylene 100mL and solid base catalyst 8.8g into the autoclave, feed CO, control the pressure to 1MPa and raise the temperature to 50°C and keep stirring for 2.5 h, CO pressure no longer drops, cool to room temperature, filter, recover the solid base catalyst, add the solvent xylene to the filtrate and divide the water layer, recover the solvent (xylene) from the organic layer, and distill the residue under reduced pressure; collect 118~121 °C (7.5 mmHg) fraction, 133.5 g of the target product N,N-ethyl dimethylaminoacrylate was obtained, the yield was 93.4%, and the HPLC content was 99.2%.

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Abstract

The invention relates to the technical field of synthesis of fine chemical intermediates, in particular to a method for synthesizing N,N-dimethylaminoethyl acrylate. The method includes: taking ethyl acetate, carbon monoxide and dimethylamine as starting materials, and reacting under the action of a solid base catalyst to generate the target product N,N-dimethylaminoethyl acrylate; the solid base catalyst is preferably a supported solid base catalyst. The invention solves the problems of difficult source of raw materials, high price, harsh process conditions, large amount of three wastes, low yield, high cost and unsuitability for industrial production in the prior art; the source of raw materials is convenient, the cost is low, the reaction conditions are friendly, and the by-products Greatly reduced, its total yield is high, the utilization rate of raw materials is high, the production cost is low and the purity is high, and it is suitable for large-scale industrialized continuous production.

Description

technical field [0001] The invention relates to the technical field of synthesis of fine chemical intermediates, in particular to a synthesis method of N,N-dimethylaminoethyl acrylate. [0002] technical background [0003] Ethyl N, N-dimethylaminoacrylate is an important organic intermediate, the English name is Ethyl N, N-dimethylaminoacrylate, the CAS number is 924-99-2, the molecular formula is C7H13NO2, and the structural formula is: [0004] [0005] There are polymerizable vinyl groups and active tertiary amino groups in its molecules, which can be used to produce cationic polymer flocculants, plastics, coatings, adhesives and daily chemicals. [0006] Ethyl N,N-dimethylaminoacrylate is an important raw material for the synthesis of quinolones, which are quinolones. Quinolones are currently the most widely used anti-infective drugs in clinical practice. Due to their advantages of broad antibacterial spectrum, strong antibacterial activity, convenient administration...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/10C07C229/30
CPCC07C227/10C07C229/30
Inventor 吴政杰顾海宁徐洪顺余永志
Owner ZHEJIANG BENLI TECH CO LTD
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