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Method for preparing 1-(2-ethoxyl)-2-imidazolone by using CO2 as raw material

A technology of imidazolinone and hydroxyethyl, which is applied in the field of preparation of cyclic urea compounds, can solve the problems of harsh reaction conditions and high cost of reaction raw materials, and achieve the effects of low raw material toxicity, simple and reliable execution route, and scientific design

Active Publication Date: 2015-08-26
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defects of high cost of reaction raw materials and harsh reaction conditions in the prior art, the purpose of the present invention is to provide a green, efficient and simple CO 2 Method for preparing 1-(2-hydroxyethyl)-2-imidazolidinone as raw material

Method used

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  • Method for preparing 1-(2-ethoxyl)-2-imidazolone by using CO2 as raw material
  • Method for preparing 1-(2-ethoxyl)-2-imidazolone by using CO2 as raw material
  • Method for preparing 1-(2-ethoxyl)-2-imidazolone by using CO2 as raw material

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Experimental program
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Effect test

Embodiment 1

[0032] with CO 2 The method for raw material preparation 1-(2-hydroxyethyl)-2-imidazolidinone, its step is:

[0033] (1) Add 0.3mol ethanolamine, 20mL ethanol and 3mmol K to the autoclave 3 PO 4 ;

[0034] (2) Pre-introduction of CO 2 , and the reaction temperature was gradually raised to 190°C, and the CO in the autoclave was adjusted to 2 Pressure to 6MPa, react for 6h under mechanical stirring;

[0035] (3) After the reaction is completed, the autoclave is cooled to room temperature, the product is taken out, and the solvent and by-product water are removed by rotary distillation;

[0036] (4) The final product 1-(2-hydroxyethyl)-2-imidazolidinone is obtained by elution through a chromatographic column, and the elution solvent of the chromatographic column is a mixture of ethanol and dichloromethane with a volume ratio of 1:6.

[0037] The yield of the above 1-(2-hydroxyethyl)-2-imidazolidinone was 66.7%.

Embodiment 2

[0039] with CO 2 The method for raw material preparation 1-(2-hydroxyethyl)-2-imidazolidinone, its step is:

[0040] (1) Add 0.3mol ethanolamine, 20mL ethanol and 3mmol Na 3 PO 4 ;

[0041] (2) Pre-introduction of CO 2 , and the reaction temperature was gradually raised to 170°C, and the CO in the autoclave was adjusted 2 Pressure to 6MPa, react for 10h under mechanical stirring;

[0042] (3) After the reaction is completed, the autoclave is cooled to room temperature, the product is taken out, and the solvent and by-product water are removed by rotary distillation;

[0043] (4) The final product 1-(2-hydroxyethyl)-2-imidazolidinone is obtained by elution through a chromatographic column, and the elution solvent of the chromatographic column is a mixture of ethanol and dichloromethane with a volume ratio of 1:4.

[0044] The yield of the above 1-(2-hydroxyethyl)-2-imidazolidinone was 58.2%.

Embodiment 3

[0046] with CO 2 The method for raw material preparation 1-(2-hydroxyethyl)-2-imidazolidinone, its step is:

[0047](1) Add 0.3mol ethanolamine, 20mL ethanol and 3mmol Li 3 PO 4 ;

[0048] (2) Pre-introduction of CO 2 , and the reaction temperature was gradually raised to 170°C, and the CO in the autoclave was adjusted 2 Pressure to 8MPa, react for 6h under mechanical stirring;

[0049] (3) After the reaction is completed, the autoclave is cooled to room temperature, the product is taken out, and the solvent and by-product water are removed by rotary distillation;

[0050] (4) The final product 1-(2-hydroxyethyl)-2-imidazolidinone is obtained by elution through a chromatographic column, and the elution solvent of the chromatographic column is a mixture of ethanol and dichloromethane with a volume ratio of 1:5.

[0051] The yield of the above 1-(2-hydroxyethyl)-2-imidazolidinone was 28.5%.

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Abstract

The invention relates to the field of preparation of cyclic urea compounds, particularly to a method for preparing 1-(2-ethoxyl)-2-imidazolone by using CO2 as a raw material. 1-(2-ethoxyl)-2-imidazolone is obtained through a reaction of CO2 and ethanolamine. Compared with a conventional technology for preparing 1-(2-ethoxyl)-2-imidazolone, the method disclosed by the invention has the following advantages: (1) a synthetic method is scientific to design, an execution route is concise and reliable, and the method is suitable for industrial production; (2) required raw materials are low in toxicity, are cheap and are easy to obtain, so that the method conforms to the trend of green chemical development; (3) a catalyst is used in the reaction process, the catalytic activity is high, and the product yield is higher; (4) from the view of resources, the CO2 is a safe non-toxic rich carbon resource, and a reaction product, namely water, does not cause pressure to the environment.

Description

technical field [0001] The invention relates to the field of preparation of cyclic urea compounds, specifically a CO 2 Process for the preparation of 1-(2-hydroxyethyl)-2-imidazolidinone as a starting material. Background technique [0002] A large amount of carbon dioxide emissions have brought serious environmental and climate problems, but carbon dioxide is also a carbon source with abundant reserves, cheap, non-toxic and recyclable, and is a potential raw material for organic chemical industry. The use of carbon dioxide for organic synthesis not only reduces the concentration of carbon dioxide in the atmosphere, but also fixes carbon dioxide as a valuable organic chemical. The invention uses amine substances to fix carbon dioxide, and successfully synthesizes a cyclic urea compound 1-(2-hydroxyethyl)-2-imidazolidinone. [0003] The CAS number of 1-(2-hydroxyethyl)-2-imidazolinone is 3699-54-5, and the structural formula is as follows: [0004] [0005] 1-(2-hydroxy...

Claims

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Application Information

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IPC IPC(8): C07D233/32
CPCC07D233/32
Inventor 赵贵哲向阳程冬冬刘亚青
Owner ZHONGBEI UNIV
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