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Preparation method of 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane

A kind of technology of methoxyphenoxy and methoxyphenol, applied in 1 field to achieve the effect of improving reaction yield

Active Publication Date: 2018-04-20
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the development of tactical high-energy solid propellants, it was found that stabilizers such as N-methyl-p-nitroaniline (MNA), which have been used in existing high-energy solid propellants (such as NEPE propellants), have strong reactivity, and can be Reacts with curing agents (isocyanates) used in tactical high-energy solid propellants, limiting MNA applications

Method used

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  • Preparation method of 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane
  • Preparation method of 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane
  • Preparation method of 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane

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Experimental program
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Embodiment 1

[0023] Under stirring at a temperature of 20°C, 13.66g (110mmol) of 4-methoxyphenol and 7.51g (50mmol) of triethylene glycol were added to 100ml of acetonitrile, and 24.72g (120mmol) of dicyclohexylcarbodiimide was added thereto. ), the temperature was raised to 85° C., and after 24 hours of reaction, the acetonitrile was distilled off under reduced pressure to obtain an orange-yellow turbid liquid 1;

[0024] Extract the above orange turbid liquid 1 with 50ml dichloromethane three times, wash three times with 50ml 1M sodium hydroxide solution, wash twice with 50ml saturated sodium chloride solution (20°C), dry over anhydrous magnesium sulfate, Dichloromethane was evaporated to dryness under normal pressure to obtain a yellow oily liquid;

[0025] Add 25ml of diethyl ether to the above yellow oily liquid, raise the temperature to 35°C, filter off the insoluble matter, cool to -15°C, cool down for 3h, filter the solution to obtain 17.86g of white powdery solid 1,2-bis(2-(4-meth...

Embodiment 2

[0032] Under stirring at a temperature of 20°C, 13.66g (110mmol) of 4-methoxyphenol and 7.51g (50mmol) of triethylene glycol were added to 100ml of acetonitrile, and 24.72g (120mmol) of dicyclohexylcarbodiimide was added thereto. ), the temperature was raised to 85° C., and after 16 hours of reaction, the acetonitrile was distilled off under reduced pressure to obtain an orange-yellow turbid liquid 1;

[0033] Extract the above orange turbid liquid 1 with 50ml dichloromethane three times, wash three times with 50ml 1M sodium hydroxide solution, wash twice with 50ml saturated sodium chloride solution (20°C), dry over anhydrous magnesium sulfate, Dichloromethane was evaporated to dryness under normal pressure to obtain a yellow oily liquid;

[0034] Add 25ml of diethyl ether to the above yellow oily liquid, raise the temperature to 35°C, filter off the insoluble matter, cool to -15°C, cool down for 3h, filter the solution to obtain 17.02g of white powdery solid 1,2-bis(2-(4-meth...

Embodiment 3

[0036] Under stirring at a temperature of 20°C, 13.66g (110mmol) of 4-methoxyphenol and 7.51g (50mmol) of triethylene glycol were added to 100ml of acetonitrile, and 24.72g (120mmol) of dicyclohexylcarbodiimide was added thereto. ), the temperature was raised to 85° C., and after 30 hours of reaction, the acetonitrile was distilled off under reduced pressure to obtain an orange-yellow turbid liquid 1;

[0037] Extract the above orange turbid liquid 1 with 50ml dichloromethane three times, wash twice with 50ml 1M sodium hydroxide solution, then wash twice with 50ml saturated sodium chloride solution (20°C), dry over anhydrous magnesium sulfate, Dichloromethane was evaporated to dryness under normal pressure to obtain a yellow oily liquid;

[0038] Add 25ml of diethyl ether to the above yellow oily liquid, raise the temperature to 35°C, filter off the insoluble matter, cool to -15°C, cool down for 3h, and filter the solution to obtain 17.94g of white powdery solid 1,2-bis(2-(4-met...

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Abstract

The invention discloses a preparation method of 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane, and aims to solve the problems that in the prior art, used reactants are not environmentally friendly, theyield is low and the like. 4-methoxyphenol and triethylene glycol are used as raw materials, and the preparation method comprises the following steps: (1), stirring at 20 DEG C, adding 4-methoxyphenoland triethylene glycol into acetonitrile, adding dicyclohexylcarbodiimide, reacting for 24h at 85 DEG C, and evaporating out acetonitrile to obtain a turbid liquid 1; (2), adding dichloromethane intothe turbid liquid 1, filtering, washing for 3 times with 1M sodium hydroxide, washing twice with saturated sodium chloride, drying by anhydrous magnesium sulfate, and evaporating out dichloromethaneto obtain a yellow powdery solid 2; (3), adding ethyl ether into the yellow powdery solid 2, raising the temperature to 35 DEG C, filtering out insolubles, cooling to -15 DEG C, lowering the temperature for 4 hours, and filtering to obtain a white powdery solid, namely 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane. The method is mainly applied to preparation of 1, 2-bis(2-(4-methoxyphenoxy)ethoxy)ethane.

Description

technical field [0001] The invention relates to a synthesis method of 1,2-bis(2-(4-methoxyphenoxy)ethoxy)ethane. It belongs to organic synthesis. Background technique [0002] The ability of a solid propellant to maintain its chemical properties during storage without exceeding the allowable variation range is called chemical stability. Commonly used nitrocellulose, nitroglycerin and other nitrate-containing compounds are the main energy components in double-base and modified double-base propellants. Decomposition will release a large amount of gas and heat, and the released nitrogen oxides will accelerate the decomposition of nitrate esters and form a self-catalyzed reaction, resulting in a decrease in the mechanical properties and combustion performance of the propellant, and even vicious accidents such as combustion and explosion. Therefore, propellants containing nitrate-based components will also decompose under storage conditions, resulting in a decrease in propellan...

Claims

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Application Information

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IPC IPC(8): C07C41/09C07C43/205
CPCC07C41/09C07C43/2055
Inventor 陆婷婷陈斌汪营磊潘永飞高福磊姬月萍张丽洁丁峰刘亚静刘卫孝闫峥峰
Owner XIAN MODERN CHEM RES INST
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