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A kind of process for preparing cryptand 222

A process method and a cave ether technology are applied in the technical field of preparing cave ether 222, which can solve the problems of low yield, long synthesis period, equipment usage fee and energy usage fee, etc., and achieves simple reaction operation, short reaction period, and high productivity. high rate effect

Active Publication Date: 2020-09-04
SUZHOU BAILINGWEI HYPERFINE MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of the fact that the above-mentioned technique for preparing cryptand 222 has long synthesis period, low yield, high equipment usage fee and energy usage fee, etc.

Method used

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  • A kind of process for preparing cryptand 222
  • A kind of process for preparing cryptand 222
  • A kind of process for preparing cryptand 222

Examples

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preparation example Construction

[0031] figure 1 It is a schematic flow diagram of the process structure of the process method for preparing cryptand 222 of the present invention, such as figure 1 As shown, the present invention provides a kind of processing method for preparing cryptand 222, wherein, comprises the following steps:

[0032] Step 1, using tris[(2-ethyleneoxy)ethyl]amine as a raw material, reacting under the catalysis of Grubbs catalyst and alkali metal salt to obtain an intermediate;

[0033]

[0034] Step 2. React the intermediate obtained in Step 1 under the catalytic action of a hydrogenation catalyst and add a hydrogen source to obtain cryptane 222.

[0035]

[0036] It should be noted that the supramolecular compound cryptane 222 prepared in the present invention can be widely used in fields such as analysis and detection, phase transfer catalysis, and life sciences.

[0037] In a further embodiment of the present invention, the Grubbs catalyst in step 1 is one or more of the firs...

example 1

[0047] Example 1 prepares the processing method of cryptand 222

[0048]This example is the process for preparing cryptand 222, comprising the steps:

[0049] Step 1: Preparation of intermediates

[0050]

[0051] In this example, this step was performed under nitrogen protection.

[0052] First, in the 20L reactor, add 10L methylene chloride, 100g sodium iodide and 3kg tris[(2-ethyleneoxy)ethyl]amine successively, stir well;

[0053] Then, 10 g of the first-generation Grubbs catalyst was added thereto, and the reaction was stirred at room temperature for 6 hours, and the reaction was completed.

[0054] Finally, the reaction solution was filtered through diatomaceous earth and alumina in sequence, and the filtrate was spin-dried to obtain a slurry-like intermediate.

[0055] Step 2: Preparation of cryptand 222

[0056]

[0057] First, stir at room temperature, add 10L of ethanol and the slurry intermediate obtained in the previous step to the 20L reaction kettle in ...

example 2

[0061] Example 2 prepares the processing method of cryptand 222

[0062] This example is the process for preparing cryptand 222, comprising the steps:

[0063] Step 1: Preparation of intermediates

[0064]

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PUM

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Abstract

The invention discloses a process method for preparing cryptand 222. The process method comprises the following steps: 1, taking tris[(2-ethylnenoxy)ethyl]amine as a raw material, and reacting to obtain an intermediate under catalytic actions of a Grubbs catalyst and alkali metal salts; and 2, adding a hydrogen source into the intermediate obtained in the step 1 under the catalytic action of a hydrogenation catalyst, and reacting, thereby obtaining the cryptand 222. The process method disclosed by the invention has the beneficial effects of short synthesis period and high yield.

Description

technical field [0001] The invention belongs to the field of preparation methods of supramolecular compound-cryptand 222, and in particular relates to a process for preparing cryptand 222. Background technique [0002] The three-dimensional internal cavity of cryptin can be closely combined with foreign ions, and the complex formed is called cryptate. The strongest binding capacity is the harder cations, including NH4 + (ammonium ion) and cations of lanthanides, alkali metals, alkaline earth metals. Cryptan utilizes the nitrogen and oxygen in the molecule to coordinate with these ions. Because different ions have different binding abilities with different three-dimensional structures of cryptin, different alkali metal cations can be distinguished or separated by selecting appropriate cryptin. [0003] However, compared with other complexing agents such as crown ethers, cryptin binds to alkali metal ions more tightly and is more selective. Through coordination, cryptin can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 龙韬陈丕证邹增龙
Owner SUZHOU BAILINGWEI HYPERFINE MATERIAL
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