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Preparation method of amino polyether (2.2.2)

An amino polyether and intermediate technology, applied in the field of preparation of amino polyether, can solve the problems of low reaction yield, long synthesis period, low yield and the like, and achieve the effect of improving the reaction yield

Active Publication Date: 2018-11-16
JIANGSU INST OF NUCLEAR MEDICINE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the applicant has found through research that when the content of sodium ions is reduced to a certain amount in the method of decomplexing by ion exchange resin, the decomplexing cannot be carried out, and the yield is low.
[0004] In view of problems such as a large number of carcinogenic toluene solvents used in the above-mentioned method for preparing aminopolyether (2.2.2), long synthesis period, and low reaction yield, a kind of aminopolyether (2.2. 2) The preparation method has very important significance

Method used

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Embodiment 1

[0027] The present embodiment provides a kind of preparation method of amino polyether (2.2.2), comprises the steps:

[0028] Step 1: Preparation of intermediate triethylene glycol bis(p-toluenesulfonate)

[0029] First, dissolve 0.45mol triethylene glycol in 200mL tetrahydrofuran, then add it to 250mL 5mol / L NaOH solution to form a mixed solution, place the mixed solution in ice water, control its temperature below 5°C, and start magnetic stirring.

[0030] Then, dissolve 1.08mol of p-toluenesulfonyl chloride in 200mL of tetrahydrofuran, and add it dropwise to the mixed solution for 1 hour. During the dropping process, the temperature is controlled below 5°C. After the dropping, stir the reaction 2h, the reaction temperature was controlled at 0-5°C.

[0031] Finally, after the reaction, the product was poured into a 500mL beaker of ice-water mixture, cooled, crystals were precipitated, filtered, washed with water, and dried to obtain a crude product; the crude product was re...

Embodiment 2

[0040] The present embodiment provides a kind of preparation method of amino polyether (2.2.2), comprises the steps:

[0041] Step 1: Preparation of intermediate triethylene glycol bis(p-toluenesulfonate)

[0042] First, dissolve 0.45mol triethylene glycol in 200mL tetrahydrofuran, then add it to 200mL 6mol / L NaOH solution to form a mixed solution, place the mixed solution in ice water, control its temperature below 3°C, and start magnetic stirring.

[0043] Then, dissolve 1.08mol of p-toluenesulfonyl chloride in 200mL of tetrahydrofuran, and add it dropwise to the mixed solution for 1.5 hours. During the dropping process, the temperature is controlled below 3°C. The reaction was carried out for 2.5 hours, and the reaction temperature was controlled at 0-3°C.

[0044] Finally, after the reaction, the product was poured into a 520mL beaker of ice-water mixture, cooled, crystals were precipitated, filtered, washed with water, and dried to obtain a crude product; the crude product...

Embodiment 3

[0051] The present embodiment provides a kind of preparation method of amino polyether (2.2.2), comprises the steps:

[0052] Step 1: Preparation of intermediate triethylene glycol bis(p-toluenesulfonate)

[0053] First, dissolve 0.45mol triethylene glycol in 200mL tetrahydrofuran, then add it to 250mL 4mol / L NaOH solution to form a mixed solution, place the mixed solution in ice water, control its temperature below 5°C, and start magnetic stirring.

[0054] Then, dissolve 0.99mol of p-toluenesulfonyl chloride in 500mL of tetrahydrofuran, and add it dropwise to the mixed solution. The dropping time is 3 hours. During the dropping process, the temperature is controlled below 5°C. After the dropping, stir the reaction 3.5h, the reaction temperature is controlled at 0-5°C.

[0055] Finally, after the reaction, the product was poured into a 650mL beaker of ice-water mixture, cooled, crystals were precipitated, filtered, washed with water, and dried to obtain a crude product; the ...

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Abstract

The invention belongs to the technical field of cryptand preparation, and concretely relates to a preparation method of amino polyether (2.2.2). The preparation method comprises the following steps: taking triglycol and paratoluensulfonyl chloride as raw materials, triethylene glycol di(p-toluenesulfonate) is obtained through a nucleophilic reaction, and then the material is subjected to a reaction with 2,2'-(ethylenedioxy)di(ethylamine), and through complexation and recrystallization, the amino polyether (2.2.2) is obtained; the reaction condition is mild and simple, a synthesis period can reduced to 27 h, the overall yield is no lower than 49%, and the method has the beneficial effects of short reaction period and high yield.

Description

technical field [0001] The invention belongs to the technical field of cryptane preparation, and in particular relates to a preparation method of amino polyether (2.2.2). Background technique [0002] Amino polyether (2.2.2) is a three-bridge crown ether molecule with a crypt cavity, a typical aza cryptate, and a type of cryptate. Due to its unique coordination characteristics, azacryptate can well select the cations of complex transition metals and heavy metals, and the generated complexes are more stable, and also have lipophilicity and hydrophilicity, so they have good research prospect. [0003] In the prior art, the classic synthesis method of amino polyether (2.2.2) is the highly diluted method proposed by Lehn et al., which is one of the typical non-template ion synthesis methods. The specific steps are, the raw material 1,8-diamino- 3,6-dioxa-octane and 1,8-diacid chloride-3,6-dioxa-octane were dissolved in a large amount of benzene solvent, and heated for 8 hours,...

Claims

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Application Information

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IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 王洪勇韩国庆邹霈刘娅灵吴军吴昊
Owner JIANGSU INST OF NUCLEAR MEDICINE
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