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A kind of synthetic method of 2'-oxydiethylamine and product thereof

A technology of oxydiethylamine and oxydiethylamine hydrochloride, applied in the field of synthesis of 2'-oxydiethylamine, can solve the problem that the product purity is not specified in detail, the synthesis and research work is not much, and the yield It can improve the purity of the product, simplify the operation process, and reduce the loss of the product.

Active Publication Date: 2022-04-12
安徽工业大学科技园有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] At present, there are not many domestic studies on its synthesis and research. In the earlier literature reports, Mei Guangquan et al. prepared the product phthaloyl by reacting phthalimide and potassium hydroxide in an ethanol solvent. Potassium imide, using dichlorodiethyl ether as a raw material and potassium phthalimide to react with diethylamine to prepare intermediate 2,2'-diphthalimide diethyl ether, Finally, by reacting with potassium hydroxide solution, 2'-oxydiethylamine was obtained through processes such as suction filtration, washing, atmospheric distillation, and pressure distillation, and the yield of 2'-oxydiethylamine was 52%. The synthesis process not only has the disadvantages of many raw materials, cumbersome operation, and low yield, but also the purity of the product is not specified in detail.

Method used

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  • A kind of synthetic method of 2'-oxydiethylamine and product thereof
  • A kind of synthetic method of 2'-oxydiethylamine and product thereof
  • A kind of synthetic method of 2'-oxydiethylamine and product thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0049] (1) Synthesis process of 2,2'-diphthalimide diethyl ether

[0050] Dissolve 300g (2.1mol) of dichlorodiethyl ether and 777g (4.2mol) of potassium phthalimide in 1500g of DMF solvent, place in a round bottom flask, heat to 65°C, and stir for 6 hours. The reaction process The solid gradually dissolves in the medium, and the solution becomes milky white, that is, the crude product solution of 2,2'-diphthalimide diethyl ether; add 10L deionized water to the above solution, stir for 2 hours, a white solid precipitates, and filter it with suction Finally, the white solid was washed three times with deionized water, and dried at 60°C for 10 h to obtain 613 g of a white solid of 2,2'-diphthalimide diethyl ether. Theoretically, 765 g should be formed, and the product yield was 613 / 765*100%=80.25%.

[0051] (2) Synthetic process of 2'-oxydiethylamine

[0052] Take 100g of dried 2,2'-diphthalimide diethyl ether and 80g of hydrazine hydrate in a 2L round bottom flask, add 1L of ...

Embodiment 2

[0054] (1) Synthesis process of 2,2'-diphthalimide diethyl ether

[0055] Add 300g (2.1mol) dichloroethyl ether, 777g (4.2mol) potassium phthalimide and 1500g DMF solvent into a 3L round bottom flask, heat to about 65°C, stir for 8 hours, and the solid gradually dissolves during the reaction , the solution turned milky white. After the reaction was completed, 10 L of deionized water was added and the reaction solution was stirred for 4 hours, and a white solid was precipitated. After suction filtration, the white solid was washed with deionized water three times, and dried at 60° C. for 10 hours. 655 g of the product 2,2'-diphthalimide diethyl ether was obtained as a white solid, and the yield was calculated to be 85.61%.

[0056] (2) Synthetic process of 2'-oxydiethylamine

[0057] Take 100g of dried 2,2'-diphthalimide diethyl ether and 80g of hydrazine hydrate in a 2L round bottom flask, add 1L of absolute ethanol solvent, stir and reflux at 75°C for 2h, the white solid di...

Embodiment 3

[0059] (1) Synthesis process of 2,2'-diphthalimide diethyl ether

[0060] Add 300g (2.1mol) dichloroethyl ether, 777 (4.2mol) potassium phthalimide and 1500g DMF solvent into a 3L round bottom flask, heat to about 65°C, stir for 12 hours, and the solid gradually dissolves during the reaction , the solution turned milky white. After the reaction was completed, 10 L of deionized water was added and the reaction solution was stirred for 2 hours, and a white solid was precipitated. After suction filtration, the white solid was washed with deionized water three times, and dried at 60° C. for 10 hours. 721 g of the product 2,2'-diphthalimide diethyl ether was obtained as a white solid, and the yield of 2,2'-diphthalimide diethyl ether was calculated to be 94.37%.

[0061] (2) Synthetic process of 2'-oxydiethylamine

[0062] Take 100g of dried 2,2'-diphthalimide diethyl ether and 80g of hydrazine hydrate in a 2L round bottom flask, add 1L of absolute ethanol solvent, stir and reflu...

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Abstract

The invention discloses a method for synthesizing 2'-oxydiethylamine and its products, which belong to the field of compound preparation. The method uses dichlorodiethyl ether as a starting material, and firstly combines potassium phthalimide with potassium phthalimide in the second place. Heating reaction in an organic solvent to generate 2,2'-diphthalimide diethyl ether, which is purified and reacted with hydrazine hydrate in a second organic solvent by heating to reflux to generate crude product 2'-oxydiethylamine After the crude product 2'-oxydiethylamine is purified, the pure product 2'-oxydiethylamine is obtained; the product yield of this method is high, the purity is high, and the controllability is strong; the product purity obtained is higher than conventional The method has been greatly improved.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a synthesis method of 2'-oxydiethylamine and a product thereof. Background technique [0002] The structural formula of 2'-oxydiethylamine is as follows: [0003] [0004] Chemical name: 2'-oxydiethylamine [0005] English name: 2,2'-oxydiethanamine [0006] CAS number: 2752-17-2 [0007] Molecular formula: C 4 h 12 N 2 o [0008] Molecular weight: 104.15 [0009] 2'-Oxydiethylamine is also known as 2,2'-oxybis(ethylamine), 2,2-oxodiethylamine; 2,2'-oxobis(ethylamine); 2,2'- Diaminodiethyl ether, 3-oxopentanediamine, 3-oxa-1,5-pentanediamine, their outstanding structural features are that the molecule contains two primary amino groups and ethoxy groups, and has strong coordination ability. It is widely used in coordination chemistry and is an important intermediate in organic synthesis. The crown ethers, open-chain and macrocyclic Schiff base l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/08C07C213/10C07C217/08
CPCC07C213/08C07C213/10C07D209/48C07C217/08
Inventor 叶明富夏国威许立信金玲宋丰发万超
Owner 安徽工业大学科技园有限公司
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