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Supported platinum complex oxidizing agent easy to recycle and preparation method and application thereof

A platinum complex and oxidant technology, which is applied in the field of supported platinum complex oxidant and its preparation, can solve the problems of inability to recycle and reuse, complicated recovery operation, etc., and achieves simple recovery and regeneration treatment, simple preparation and high yield. Effect

Inactive Publication Date: 2018-04-10
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the purposes of the present invention is to provide a load-type platinum complex oxidant that is easy to recycle and use and its application, so as to solve the problem that the existing platinum complex oxidant cannot be recycled or reused when it is used to synthesize disulfide bonds in polypeptide molecules. complicated question

Method used

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  • Supported platinum complex oxidizing agent easy to recycle and preparation method and application thereof
  • Supported platinum complex oxidizing agent easy to recycle and preparation method and application thereof
  • Supported platinum complex oxidizing agent easy to recycle and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0051] The polystyrene microspheres used in this example are commercially available, with a particle size of 110 μm.

[0052] ①In a 250 mL three-necked flask, add 1.0 g of polystyrene microspheres and 100 mL of anhydrous pyridine, then add 5 g of p-toluenesulfonyl chloride, stir magnetically, and react at room temperature for 3 days; after the reaction is completed, filter and wash the obtained solid with ethanol 5 times, then 50 o C vacuum drying 12h, obtains the polystyrene microsphere of p-toluenesulfonyl modification of yellow;

[0053] ②Add 1.0g p-toluenesulfonyl-modified polystyrene microspheres into a 100mL three-necked flask, then add 50mL ethylenediamine, stir with magnetic force, 60 o C reaction 2d; after the reaction is completed, filter, and wash the solid with ethanol 3 times, then vacuum-dry to obtain dark yellow ethylenediamine-modified polystyrene microspheres;

[0054] ③Weigh 0.2g of ethylenediamine-modified polystyrene microspheres into a 100mL three-neck f...

Embodiment 2

[0059] The polystyrene microspheres used in this example are commercially available, with a particle size of 75 μm.

[0060] ①In a 250 mL three-necked flask, add 1.0 g of polystyrene microspheres and 100 mL of anhydrous pyridine, then add 5 g of p-toluenesulfonyl chloride, stir magnetically, and react at room temperature for 2 days; after the reaction is completed, filter and wash the obtained solid with ethanol for 5 times, then 50 o C vacuum drying 12h, obtains the polystyrene microsphere of p-toluenesulfonyl modification of yellow;

[0061] ②Add 1.0g p-toluenesulfonyl-modified polystyrene microspheres into a 100mL three-necked flask, then add 50mL ethylenediamine, stir with magnetic force, 60 o C reaction 1d; after the reaction is completed, filter, wash the solid 3 times with ethanol, and then vacuum-dry to obtain dark yellow ethylenediamine-modified polystyrene microspheres;

[0062] ③Weigh 0.2g of ethylenediamine-modified polystyrene microspheres into a 100mL three-nec...

Embodiment 3

[0065] The polystyrene microspheres used in this example are commercially available, with a particle size of 320 μm.

[0066] ①In a 250 mL three-necked flask, add 1.0 g polystyrene microspheres and 150 mL anhydrous pyridine, then add 5 g p-toluenesulfonyl chloride, stir magnetically, and react at room temperature for 3 days; after the reaction is completed, filter and wash the obtained solid with ethanol for 5 times, then 50 o C vacuum drying 12h, obtains the polystyrene microsphere of p-toluenesulfonyl modification of yellow;

[0067] ②Add 1.0g p-toluenesulfonyl-modified polystyrene microspheres into a 100mL three-neck flask, then add 80mL ethylenediamine, stir with magnetic force, 80 o C reaction 2d; after the reaction is completed, filter, and wash the solid with ethanol 3 times, then vacuum-dry to obtain dark yellow ethylenediamine-modified polystyrene microspheres;

[0068] ③Weigh 0.2g of ethylenediamine-modified polystyrene microspheres into a 100mL three-neck flask, a...

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Abstract

The invention discloses a supported platinum complex oxidizing agent easy to recycle. The supported platinum complex oxidizing agent is provided with the structure shown in the formula I. The invention further provides a preparation method of the oxidizing agent. The method comprises the steps that 1, pyridine is taken as solvent, and polystyrene microsphere is reacted with toluene sulfonyl chloride to obtain a yellow solid substance; 2, ultrasonic dispersion is conducted on the obtained yellow solid substance in ethylenediamine, and the yellow solid substance is subjected to stirring reactionto obtain a deep yellow solid substance; 3, DMF is taken as solvent, and the obtained deep yellow solid substance and a two-valence platinum complex are subjected to stirring reaction to obtain a black solid substance; 4, after ultrasonic dispersion is conducted on the black solid substance in ethyl alcohol, the black solid substance is fully reacted with N,N'-bromosuccinimide to obtain a light black solid substance, namely the supported platinum complex oxidizing agent. The oxidizing agent preparation method is simple, recycle is easy, and the reaction yield is high.

Description

technical field [0001] The invention relates to a supported platinum complex oxidant, in particular to a supported platinum complex oxidant which is easy to recycle and use, its preparation method and application. Background technique [0002] The disulfide bond in the polypeptide molecule is an important functional group to maintain the high-order conformation of the polypeptide and improve the physiological and pharmacological activities of the polypeptide. The disulfide bond in the drug polypeptide molecule can improve the stability and permeability of the drug molecule in the body, and increase the specific binding between the drug molecule and the target molecule, thereby improving the biological activity of the polypeptide drug ( Nature Chem. , 2014, 6 ,1009–1016; Chem. Rew. , 2013, 114 , 901–926.). Many peptide drugs containing intramolecular disulfide bonds have been approved by the FDA and used to treat various diseases, such as: octreotide for the treatment of...

Claims

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Application Information

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IPC IPC(8): C07K1/00
CPCC07K1/00
Inventor 霍树营宋常英张亚梅侯晓男申世刚
Owner HEBEI UNIVERSITY
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