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Synthesis method of 1,2-di(2-(4-dimethoxyphenoxy) ethoxy) ethane

A technology of dimethoxyphenoxy and methoxyphenoxy, which is applied in the field 1, can solve the problems of complex post-processing and long reaction time, and achieve the effect of simple post-processing and increasing reaction yield

Inactive Publication Date: 2018-04-13
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The reaction time of the Pursiainen method is longer, and the post-processing is more complicated. The characterization data given by Pursiainen in the article has a big problem. The number of Hs shown in 1H NMR is 30, but the actual number of Hs in this compound is 24. , the yield of Pursiainen method is 96%

Method used

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  • Synthesis method of 1,2-di(2-(4-dimethoxyphenoxy) ethoxy) ethane
  • Synthesis method of 1,2-di(2-(4-dimethoxyphenoxy) ethoxy) ethane
  • Synthesis method of 1,2-di(2-(4-dimethoxyphenoxy) ethoxy) ethane

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Experimental program
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Embodiment 1

[0025] Under stirring at a temperature of 20°C, 13.66g (110mmol) of 4-methoxyphenol and 9.30g (50mmol) of 1,2-(dichloroethane)ethane were added to 100ml of N,N-dimethylformamide, Add 6.72g (120mmol) of potassium hydroxide to it, react at 150°C for 12h, pour the reaction liquid into water to obtain brown turbid liquid 1;

[0026] Cool the above brown turbid liquid 1 to -15°C for 4h, filter the solution to obtain a white flake solid, add ether to the white flake solid, heat to 35°C, filter out insolubles, cool to -15°C, keep for 4h , The solution was filtered to obtain 17.92 g of white powdery solid 1,2-bis(2-(4-dimethoxyphenoxy)ethoxy)ethane. The yield is 98.35%, the purity is 98.11%, and the melting point is 67-68°C.

[0027] Structure Identification:

[0028] IR(KBr)ν:3444,3057,3014,2959,2931,2902,2871,2838,2786,2700,2590,2545,

[0029] 2474,2345,2125,2050,1986,1905,1866,1740,1626,1509,1453,1385,1332,1287,1250,

[0030] 1229,1189,1132,1116,1072,1055,1031,948,927,883,821,731,593,522,...

Embodiment 2

[0035] Under stirring at a temperature of 20°C, 13.66g (110mmol) of 4-methoxyphenol and 9.30g (50mmol) of 1,2-(dichloroethane)ethane were added to 100ml of N,N-dimethylformamide, 6.72g (120mmol) of potassium hydroxide was added thereto, reacted at 130°C for 12h, and the reaction solution was poured into water to obtain brown turbid liquid 1;

[0036] Cool the above brown turbid liquid 1 to -15°C for 4h, filter the solution to obtain a white flake solid, add ether to the white flake solid, heat to 35°C, filter out insolubles, cool to -15°C, keep for 4h , The solution was filtered to obtain 17.63 g of white powdery solid 1,2-bis(2-(4-dimethoxyphenoxy)ethoxy)ethane. The yield is 96.76%, the purity is 98.06%, and the melting point is 67-68°C.

Embodiment 3

[0038] Under stirring at a temperature of 20°C, 13.66g (110mmol) of 4-methoxyphenol and 9.30g (50mmol) of 1,2-(dichloroethane)ethane were added to 100ml of N,N-dimethylformamide, 6.16g (110mmol) of potassium hydroxide was added thereto, reacted at 150°C for 12h, and the reaction solution was poured into water to obtain brown turbid liquid 1;

[0039] Cool the above brown turbid liquid 1 to -15°C for 4h, filter the solution to obtain a white flake solid, add ether to the white flake solid, heat to 35°C, filter out insolubles, cool to -15°C, keep for 4h , The solution was filtered to obtain 17.25 g of white powdery solid 1,2-bis(2-(4-dimethoxyphenoxy)ethoxy)ethane. The yield is 94.68%, the purity is 98.13%, and the melting point is 67-68°C.

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Abstract

The invention discloses a synthesis method of 1,2-di(2-(4-methoxyphenoxy) ethoxy) ethane, and aims to solve the problems of long reaction time, complex post-treatment and the like in the prior art. According to the method provided by the invention, 4-methoxyphenol and 1,2-(dichloroethane group) ethane are taken as raw materials, and the method comprises the following steps: (1) carrying out stirring at 20 DEG C, adding 4-methoxyphenol and 1,2-(dichloroethane group) ethane into N,N-dimethylformamide, adding potassium hydroxide to react at 150 DEG C for 12h, and pouring a reaction solution intowater to obtain a brown turbid solution 1; (2) cooling the brown solution 1 to -15 DEG C, keeping the temperature for 4h, filtering the brown solution to obtain a white flaky solid, adding diethyl ether into the white flaky solid, raising the temperature to 35 DEG C, filtering the mixture when the mixture is hot, cooling the mixture to -15 DEG C, keeping the temperature for 4h, and carrying out filtering to obtain white powdery solid 1,2-di(2-(4-dimethoxyphenoxy) ethoxy) ethane. The method provided by the invention is mainly used for synthesizing 1,2-di(2-(4-dimethoxyphenoxy) ethoxy) ethane.

Description

Technical field [0001] The invention relates to a synthesis method of 1,2-bis(2-(4-dimethoxyphenoxy)ethoxy)ethane. It is organic synthesis. Background technique [0002] The ability of a solid propellant to keep its chemical properties within the allowable range during storage is called chemical stability. Commonly used nitrocellulose, nitroglycerin and other nitrate ester-containing compounds are the main energy components in double-base and modified double-base propellants. The nitrate ester bond is easy to break (bond energy 150.5-167.2kJ / mol), which generates heat Decomposition releases a large amount of gas and heat, and the released nitrogen oxides accelerate the decomposition of nitrate esters to form an autocatalytic reaction, which leads to the decline of the mechanical properties and combustion performance of the propellant, and even combustion, explosion and other vicious accidents. Therefore, the propellant containing nitrate ester-based components will also decompo...

Claims

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Application Information

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IPC IPC(8): C07C41/18C07C41/16C07C43/205
CPCC07C41/16C07C41/18C07C43/2055
Inventor 陆婷婷高福磊丁峰刘亚静汪营磊闫峥峰刘卫孝张丽洁姬月萍陈斌潘永飞
Owner XIAN MODERN CHEM RES INST
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