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Method for preparing fully-substituted calix [8] aromatic phosphate derivative

An aromatic phosphate ester, full substitution technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. problem, to achieve the effect of easy purification, simple synthesis route and high reaction yield

Inactive Publication Date: 2016-03-09
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] This patent aims at the problems of complex synthesis routes, low yields and incomplete substitution of derivatives in general synthesis methods, and proposes a method for synthesizing completely substituted calix[8]arene phosphate derivatives in one step using cheap and easy-to-obtain raw materials

Method used

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  • Method for preparing fully-substituted calix [8] aromatic phosphate derivative
  • Method for preparing fully-substituted calix [8] aromatic phosphate derivative
  • Method for preparing fully-substituted calix [8] aromatic phosphate derivative

Examples

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Effect test

Synthetic example 1

[0020] Take 4g (3mmol) of p-tert-butylcalix[8]arene, 8.58g (60mmol) of dimethyl chlorophosphate, 0.4g of tetrabutylammonium bromide (TBAB) and 200ml of dichloromethane (DCM), and mix well with electromagnetic stirring , 100ml of 50% aqueous sodium hydroxide solution was slowly dripped into the reaction system, the temperature of the reaction system was raised to reflux, and the reaction progress was detected by thin-layer chromatography until the reaction was complete.

[0021] After the reaction was completed, the organic layer was separated, washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, the residue was dissolved in methanol, precipitated with water, filtered, the filter cake was dissolved in ether and washed with water, the organic layer was dried with anhydrous sodium sulfate, and the solvent was evaporated to obtain a white solid a with a yield of 92 %, its product purity is greater than 95%.

Synthetic example 2

[0023] The synthesis method is similar to Synthesis Case 1, take 4g (3mmol) calix[8]arene, 10.32g (60mmol) diethyl chlorophosphate, 0.4g tetrabutylammonium bromide (TBAB) and 200ml dichloromethane (DCM) to add Put it into a 500ml three-neck flask, stir it evenly with electromagnetic stirring, slowly drop 100ml of 50% sodium hydroxide aqueous solution into the reaction system, raise the temperature of the reaction system to reflux, and detect the reaction progress by thin-layer chromatography until the reaction is complete. After the reaction was completed, it was washed with saturated brine and water. After purification, it was white powder b with a yield of 90%.

Synthetic example 3

[0025] The synthesis method is similar to Synthesis Case 1, take 4g (3mmol) calix[8]arene, 12g (60mmol) diethyl chlorophosphate, 0.4g tetrabutylammonium bromide (TBAB) and 200ml dichloromethane (DCM) into In a 500ml three-neck flask, electromagnetically stir and mix evenly, slowly drop 100ml of 50% sodium hydroxide aqueous solution into the reaction system, raise the temperature of the reaction system to reflux, and detect the reaction progress by thin-layer chromatography until the reaction is complete. After the reaction was completed, it was washed with saturated brine and water. After purification, it was a white powder c with a yield of 86%.

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Abstract

The present invention describes a method for preparing a fully-substituted calix [8] aromatic phosphate derivative. In the method, calix [8] aromatic is used as a parent, and by use of the characteristics that 8 phenolic hydroxyl groups of the lower edge of the calixarene can be modified functionally under alkaline conditions, the fully-substituted calix [8] aromatic phosphate derivative is prepared by one-step method. The new fully-substituted calix [8] aromatic phosphate derivative can be used to improve the separation efficiency and the selectivity of rare earth ions. The method is high in yield, convenient in purification, mild in conditions, complete in substitution, and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing fully substituted calix[8]arene phosphate derivatives, in particular, the complete substitution of eight OH groups at the lower edge of the parent calix[8] is realized. Background technique [0002] Calixarene is a kind of macrocyclic compound produced by phenolic condensation reaction. It has the advantages of adjustable cavity, variable conformation, and easy modification. It can use non-covalent It is known as the "third generation supramolecule" to recognize the guest molecule through bond interaction. The unique cavity structure of this kind of derivatives has high selectivity and affinity for certain metal ions, organic anions and cations, neutral molecules, etc., and has important applications in the fields of molecular recognition and chemical sensors. In recent years, calix[8]arenes have developed towards functionalization, that is, using calixarene as the backbone, the phenolic hydroxyl groups ...

Claims

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Application Information

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IPC IPC(8): C07F9/12
CPCC07F9/12
Inventor 梁恩湘刘湘枝易健民
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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