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Method for efficiently separating cucurbit [n] uril

A gourd, high-efficiency technology, applied in the field of high-efficiency separation of cucurbit [n] urea, can solve the problems of low product yield, long separation time, complicated separation process, etc., and achieve the effect of high separation efficiency, short separation time and simple separation process

Active Publication Date: 2020-09-01
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In view of the above problems, the object of the present invention is to provide a method for efficiently separating cucurbit [n] urea, which aims to solve the problems of long separation time, complicated separation process and low product yield in the existing separation process of cucurbit [n] urea. technical problem

Method used

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  • Method for efficiently separating cucurbit [n] uril
  • Method for efficiently separating cucurbit [n] uril
  • Method for efficiently separating cucurbit [n] uril

Examples

Experimental program
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Effect test

Embodiment

[0037] The cucurbit [n] urea mixture is dissolved in water, and then separated and purified to obtain a cucurbit [5, 7] urea mixture with better water solubility and a cucurbit [6, 8] urea mixture with poor water solubility.

[0038] Dissolve the separated cucurbit [5, 7] urea mixture in formic acid to make a saturated solution, add acetone of 1 times the volume of the formic acid solution to it while stirring, precipitate and filter with suction, the obtained precipitate is first washed with formic acid: acetone = 1:1 mixed solvent washing, then washing with acetone and drying, the obtained white solid is high-purity cucurbit [7] urea.

[0039] Add 2 times the volume of formic acid solution in acetone to the filtrate obtained by suction filtration, precipitate out and filter with suction, spin the filtrate to concentrate and precipitate with acetone, then wash and dry the precipitate with acetone, and the obtained white solid is high-purity gourd [ 5] Urea.

[0040] Dissolve...

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Abstract

The invention is applicable to the field of host-guest chemistry in supramolecular chemistry, and provides a method for efficiently separating cucurbit [n] uril. The method comprises the following steps: dissolving a cucurbit [n] uril mixture in water, and carrying out separation and purification to obtain a cucurbit [5, 7] uril mixture with good water solubility and a cucurbit [6, 8] uril mixturewith poor water solubility; and efficiently separating and purifying the cucurbituril homolog by utilizing different solubility of different cucurbiturils in a mixed solvent of formic acid and acetone. The method has the characteristics of simple separation process, short separation time, high separation efficiency, less separation loss and pure separation product.

Description

technical field [0001] The invention belongs to the field of host-guest chemistry in supramolecular chemistry, and in particular relates to a method for efficiently separating cucurbit [n] urea. Background technique [0002] Cucurbit[n]uril (CB[n]) is a macrocyclic main compound composed of n glycoluril units bridged by 2n methylene groups ( figure 1 ). Its structure is similar to squash (cucurbitaceae), so it is called cucurbituril, also called melon ring. It has a cavity open at both ends, the cavity is composed of non-polar alkyl chains, and the port is composed of polar urea carbonyl groups. The two ports have the same size and are smaller than the diameter of the cavity. With the increase of the number of glycoluril units in cucurbituril, the port diameter, cavity diameter, outer diameter and cavity volume of cucurbituril gradually increased, but the height of cucurbit[5-8]uril was consistent (Table 1). [0003] Table 1 Structural parameters of cucurbit [5-8] urea ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 王雯静周琼波周晓海王晓强
Owner WUHAN UNIV OF SCI & TECH
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