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Reaction process and device for continuously synthesizing 18-crown ether-6

A technique and technology of crown ethers, which are applied in the field of reaction techniques and devices for continuous synthesis of 18-crown ether-6, can solve the problems of high energy consumption, low yield, and difficult availability of intermediates in the intermittent operation of the synthesis process, and achieve production High efficiency, increased output, and labor-saving effects

Active Publication Date: 2022-02-11
润峙之微流体科技(江苏)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] For this reason, the embodiment of the present invention provides a reaction process and device for continuously synthesizing 18-crown-6, which mainly solves the problem of high energy consumption and low yield in the intermittent operation of the existing synthesis process or that some process intermediates are not easy to obtain and require additional synthetic problem

Method used

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  • Reaction process and device for continuously synthesizing 18-crown ether-6
  • Reaction process and device for continuously synthesizing 18-crown ether-6
  • Reaction process and device for continuously synthesizing 18-crown ether-6

Examples

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Embodiment 1

[0033] Such as image 3 Shown, at room temperature, with triethylene glycol, acid agent triethylamine molar ratio is 1:2 and solvent (the THF concentration of triethylene glycol substrate after mixing is 4 mol / liter) from feeding tank 100 and The addition tank 200 is added to the mixer 300 with electromagnetic or mechanical stirring and mixed to prepare the first premix;

[0034] In addition, at room temperature, p-toluenesulfonyl chloride (with the substrate triethylene glycol molar ratio of 2:1) and the solvent THF were mixed into a second premixture with a concentration of 8 mol / L;

[0035] With triethylene glycol, alkali potassium hydroxide molar ratio is 1:2 and solvent (the dioxane concentration of triethylene glycol substrate after mixing is 4 mol / liter) joins from feed tank 100 and feed tank 200 to following Mix in the mixer 300 of electromagnetic or mechanical agitation, make the 3rd premix;

[0036] Such as figure 1 As shown, at room temperature, the first premix ...

Embodiment 2

[0038] The difference with embodiment 1 is:

[0039] Such as figure 2 As shown, at room temperature, the first premix and the second premix are input to the micro-mixer 10 through the pump 51 and the pump 52 respectively, and the volume flows of the first premix and the second premix are respectively 10.0 mL / min and 10.0mL / min, the total volume flow rate is 20.0mL / min. The mixer 10 is an interdigitated micro-mixer with a channel size of 85 microns. Before entering the second micro-mixer 30, at first through the micro-reactor 20 to carry out sufficient esterification reaction site to generate the corresponding diol tosylate, then the mixture and the 3rd pre-mixture through the pump 61 in the micro-reactor 20 Mixing is carried out in the mixer 30 and subsequent serial etherification and cyclization reactions take place. The feed volume flow rate of each material remains the same, and the configuration of the mixer and the reactor is also unchanged. Reactor 20 is a flat-tube...

Embodiment 3

[0041] The difference with embodiment 2 is:

[0042] Such as image 3 As shown, at room temperature, the molar ratio of triethylene glycol and alkali potassium hydroxide is 1:2 and solvent (the dioxane concentration of the triethylene glycol substrate after mixing is 4 mol / liter), and a catalytic amount of 18-Crown ether-6 (molar ratio of 1:100 to the substrate diol) is added from the feed tank 100 and the feed tank 200 to the mixer 300 with electromagnetic or mechanical stirring and mixed to prepare the third pre-mixture;

[0043] Such as figure 2 As shown, the feed volume flow rate of each material remains the same, and the configuration of the mixer and the reactor is also unchanged. The crude reaction product was desalted, separated, extracted, solvent evaporated, and the crude product was distilled under reduced pressure to obtain 18-crown-6 with a yield of 76% and a total residence time of 7.5 min.

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Abstract

The invention discloses a reaction process and device for continuously synthesizing 18-crown ether-6, and particularly relates to the field of crown ether. The reaction process comprises the steps: step 1, generating corresponding methyl benzene sulfonic acid dihydric alcohol ester or methanesulfonic acid dihydric alcohol ester on site through dihydric alcohol I and paratoluensulfonyl chloride or methanesulfonyl chloride; and step 2, directly carrying out cyclization reaction on the intermediate without separation and purification and corresponding dihydric alcohol II under the action of a potassium ion template to synthesize a target product. The problems of high intermittent operation energy consumption and low yield of an existing synthesis process or the need of additional synthesis due to difficulty in obtaining of intermediates in some processes are mainly solved. According to the invention, the continuous micro-channel process can be adopted to replace an existing intermittent stirring mode, so that the cost can be substantially reduced, the energy can be saved, the yield can be improved, and the rapid amplification can be achieved so as to be suitable for industrial production.

Description

technical field [0001] The embodiment of the present invention relates to the field of crown ether synthesis, in particular to a reaction process and device for continuous synthesis of 18-crown ether-6. Background technique [0002] Crown ether is a macrocyclic polyether containing multiple -oxygen-methylene-structural units in the molecule. When naming, the total number of atoms contained in the ring is marked before the word "crown", and the number of oxygen atoms contained in it is marked in the name. after. Common crown ethers include 12-crown-4, 15-crown-5, 18-crown-6, 24-crown-8 and 30-crown-10, etc., which were accidentally discovered by Pedersen of DuPont in 1967, and It is found that this kind of compound has many unusual characteristics. The hole structure of crown ether has a selective effect on ions, and it can be used as a catalyst in organic reactions. At present, there are hundreds of crown ethers that have been synthesized, but only 30 kinds have been actua...

Claims

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Application Information

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IPC IPC(8): C07D323/00B01J19/00B01F33/30B01F33/81
CPCC07D323/00B01J19/0093
Inventor 赵东波孙尧周丽华江定春孟晓禹
Owner 润峙之微流体科技(江苏)有限公司
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