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Preparation method of 15-crown 5-ether

A technology of crown ether and dichloroethyl ether, applied in the field of preparation of 15-crown ether-5, can solve problems such as not seen, and achieve the effects of low cost, safe process operation and high yield

Active Publication Date: 2014-12-24
KENTE CATALYSTS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 15-Crown ether-5 is an important high-efficiency phase transfer catalyst, and its efficient production method has not yet been described in relevant patents and literature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of preparation method of 15-crown ether-5, carries out according to the following steps:

[0025] Step 1: Open and close the relevant valves and buttons according to the operation steps of the vacuum system, pump 240 kg of triethylene glycol and 1200 kg of dioxane into a 3000L stainless steel reactor, stir for 5 minutes to make the mixture even;

[0026] Step 2: Pump 600 kg of dichloroethyl ether and 330 kg of dioxane into the high-level tank. After the pumping, close the vacuum system first, and then open each relevant valve to make the entire reaction system a reflux device. closure;

[0027] Step 3, stop stirring the triethylene glycol and dioxane in the step 1, open the manhole cover, slowly add 190 kilograms of sodium hydroxide in the 3000L stainless steel reactor, and close the manhole cover after adding;

[0028] Step 4, start stirring, and after about 5 minutes, after the temperature of the entire reaction system is constant, slowly add steam to 60°C and...

Embodiment 2

[0036] A kind of preparation method of 15-crown ether-5, carries out according to the following steps:

[0037] Step 1: Open and close the relevant valves and buttons according to the operation steps of the vacuum system, pump 240 kg of triethylene glycol and 1200 kg of dioxane into a 3000L stainless steel reactor, stir for 5 minutes to make the mixture even;

[0038] Step 2, pump 600 kg of dichloroethyl ether and 330 kg of dioxane into the high-level tank. After the pumping, close the vacuum system first, and then open each relevant valve to make the entire reaction system a reflux device. closure;

[0039] Step 3, stop stirring the triethylene glycol and dioxane in the step 1, open the manhole cover, slowly add 190 kilograms of sodium hydroxide in the 3000L stainless steel reactor, and close the manhole cover after adding;

[0040] Step 4, start stirring, and after about 5 minutes, after the temperature of the entire reaction system is constant, slowly add steam to 60°C and...

Embodiment 3

[0048] A kind of preparation method of 15-crown ether-5, carries out according to the following steps:

[0049] Step 1: Open and close the relevant valves and buttons according to the operation steps of the vacuum system, pump 240 kg of triethylene glycol and 1200 kg of dioxane into a 3000L stainless steel reactor, stir for 5 minutes to make the mixture even;

[0050] Step 2, pump 600 kg of dichloroethyl ether and 330 kg of dioxane into the high-level tank. After the pumping, close the vacuum system first, and then open each relevant valve to make the entire reaction system a reflux device. closure;

[0051]Step 3, stop stirring the triethylene glycol and dioxane in the step 1, open the manhole cover, slowly add 190 kilograms of sodium hydroxide in the 3000L stainless steel reactor, and close the manhole cover after adding;

[0052] Step 4, start stirring, and after about 5 minutes, after the temperature of the entire reaction system is constant, slowly add steam to 60°C and ...

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PUM

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Abstract

The invention relates to a preparation method of 15-crown 5-ether, which comprises the following steps: uniformly stirring triglycol and dioxane in a reaction vessel; adding sodium hydroxide and stirring, heating to 40-60 DEG C; adding a mixed liquor of dichloroethyl ether and dioxane at the temperature lower than 60 DEG C, reacting for 20-24 hours at the temperature of 60-90 DEG C; cooling to room temperature, centrifuging to obtain a filtrate; pumping the filtrate into the reaction vessel and distilling to obtain a distillation substrate; moving the distillation substrate to a stainless steel still, performing vacuum rectification, removing primary fraction to obtain the product. The preparation method has the beneficial effect that comparing with the prior art, the preparation method has the advantages of safe operation, low cost, little three wastes and high yield, and the primary fraction in the reaction can be reutilized.

Description

technical field [0001] The invention relates to a preparation method of crown ether, in particular to a preparation method of 15-crown ether-5. Background technique [0002] The molecular formula of 15-crown-5 is C 10 h 20 o 5 , molecular weight 220.27, colorless transparent viscous liquid, easy to absorb moisture; miscible with water, soluble in ethanol, benzene, chloroform, methylene chloride and other organic solvents; strong selective complexation for sodium ions, is a high-efficiency phase Transfer catalyst, complexing agent. [0003] The application of phase transfer catalyst is a new technology developed in the past 20 years, because it overcomes the disadvantage of requiring polar aprotic solvents in heterogeneous organic synthesis, and can make heterogeneous reactions proceed under relatively mild conditions , to speed up the reaction rate and increase the yield, thus playing a great role in promoting the development of organic synthesis. [0004] 15-crown-5 is...

Claims

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Application Information

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IPC IPC(8): C07D323/00
CPCC07D323/00
Inventor 项飞勇
Owner KENTE CATALYSTS INC
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