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Preparation method of bi-(2-dimethylamino ethyl)ether

A dimethylaminoethyl and chloroethyl technology is applied in the preparation of aminohydroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc., and can solve harsh reaction conditions, high cost, unsatisfactory product yield and purity, etc. problem, to achieve the effect of mild reaction conditions, high product yield and purity

Active Publication Date: 2014-07-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] In the above-mentioned preparation methods, either it needs to be carried out under high temperature and high pressure, and the reaction conditions are harsh; or the post-treatment of the product is complicated and the cost is high; or the yield and purity of the product are not ideal

Method used

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  • Preparation method of bi-(2-dimethylamino ethyl)ether
  • Preparation method of bi-(2-dimethylamino ethyl)ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 300 g of trimethylamine aqueous solution with a content of 33 wt % and 120 g of bis(2-chloroethyl) ether into the reaction flask for reaction, raise the temperature to 70° C. for 5 hours to generate diquaternary ammonium chloride, raise the temperature to 100° C. and reduce pressure Remove water, add 440g of triphenylphosphine to the obtained product under the protection of nitrogen, heat up to 160°C for 10h, and obtain the product bis(2-dimethylaminoethyl)ether and methyltriphenylphosphonium chloride, stand still, The upper liquid layer was separated, and the liquid layer was distilled under reduced pressure to obtain two (2-dimethylaminoethyl) ethers with a content of 98% and a yield of 85%; methyltriphenylphosphonium chloride was passed through a mixed solvent of ethanol and ethyl acetate Recrystallization and purification.

Embodiment 2

[0030] Add 1000 g of trimethylamine aqueous solution with a content of 33 wt % and 400 g of bis(2-chloroethyl) ether into the reaction flask for reaction, raise the temperature to 80° C. and react for 8 hours to generate diquaternary ammonium chloride, and raise the temperature to 100° C. to reduce pressure Remove water, add 1450g of triphenylphosphine to the obtained product under the protection of nitrogen, heat up to 160°C for 8 hours, and obtain the product bis(2-dimethylaminoethyl)ether and methyltriphenylphosphonium chloride, stand still, The upper liquid layer was separated, and the liquid layer was distilled under reduced pressure to obtain two (2-dimethylaminoethyl) ethers with a content of 99% and a yield of 88%; methyltriphenylphosphonium chloride was passed through a mixed solvent of ethanol and ethyl acetate Recrystallization and purification.

Embodiment 3

[0032] Add 1000 g of trimethylamine ethanol solution with a content of 33 wt % and 400 g of bis(2-chloroethyl) ether into the reaction flask, heat up to 75°C for 10 hours to generate diquaternary ammonium chloride, and raise the temperature to 80°C to remove Ethanol, the resulting product was added under nitrogen protection, 1450g triphenylphosphine was added, the temperature was raised to 160°C for 10h, and the product bis(2-dimethylaminoethyl) ether and methyl triphenylphosphonium chloride were obtained. The upper liquid layer was removed, and the liquid layer was distilled under reduced pressure to obtain two (2-dimethylaminoethyl) ethers with a content of 99% and a yield of 84%; Crystallization and purification.

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Abstract

A method for preparing bis(2-dimethylaminoethyl)ether, comprising: under the protection of an inert gas, combining a bisquaternary ammonium salt with a structure as shown in formula (1) and a trihydrocarbyl phosphine between 100°C and 180°C React for at least 3 hours; X in formula (1) 1 and x 2 for halogen. The method of the invention has the characteristics of mild reaction conditions, high product yield and high purity.

Description

technical field [0001] The invention relates to a preparation method of bis(2-dimethylaminoethyl) ether. Background technique [0002] Bis(2-dimethylaminoethyl)ether is one of the important amine catalysts in the polyurethane industry, and its chemical structural formula is The pure product is a colorless liquid with a boiling point of 190°C. Bis(2-dimethylaminoethyl) ether has extremely high catalytic activity and selectivity for foaming reaction, and is currently widely used in the production of high resilience and cold curing polyurethane flexible foam. [0003] As early as the 1960s, foreign countries have begun to develop bis(2-dimethylaminoethyl) ether. At present, a variety of synthetic routes have been formed, mainly including: [0004] (1) under the effect of thionyl chloride, use N, N-dimethylaminoethoxy sodium and N, N-dimethylethanolamine to react to prepare two (2-dimethylaminoethyl) ethers, the productive rate is about 50%. [0005] (2) under the effect of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/08C07C213/02C07F9/54
Inventor 余伟发王秀李本高
Owner CHINA PETROLEUM & CHEM CORP
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