Reusable load type platinum complex oxidizing agents, and preparation method and application thereof

A platinum complex and oxidant technology, applied in the field of supported platinum complex oxidant and its preparation, can solve problems such as inability to recycle and reuse, and achieve the effects of simple recovery and regeneration, simple preparation, and high yield

Inactive Publication Date: 2015-11-25
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 recyclable supported platinum complex oxidant and its application, so as to solve the problem that the existing platinum complex oxidant cannot be recycled and reused when it is used to synthesize disulfide bonds in polypeptide molecules

Method used

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  • Reusable load type platinum complex oxidizing agents, and preparation method and application thereof
  • Reusable load type platinum complex oxidizing agents, and preparation method and application thereof
  • Reusable load type platinum complex oxidizing agents, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The silica microspheres used in this example are commercially available, with a particle size of 500 nm.

[0055] ①In a 250mL three-necked flask, add 2.0g of silica microspheres and 150mL of anhydrous toluene, then add 5g of N-(aminoethyl)-?-aminopropyltrimethoxysilane, magnetically stir, 120 o C reflux reaction for 48h; after completion of the reaction, cool to room temperature, filter, and the resulting solid is washed 3 times with ethanol, and then 50 o C vacuum drying 12h, obtains the silica microspheres of white ethylenediamine modification;

[0056] ②Add 1.5g of ethylenediamine-modified silica microspheres into a 250mL three-neck flask, then add 100mL of water, and add 0.3g of cis-Pt(en)Cl after ultrasonic dispersion 2 , stirring, 50 o C was reacted for 20 h; after the reaction was completed, it was cooled to room temperature, filtered, and the solid was washed 3 times with ethanol, and then dried in vacuo to obtain off-white silica microspheres loaded with diva...

Embodiment 2

[0062] The silica microspheres used in this example are commercially available, with a particle size of 100 nm.

[0063] ①In a 250mL three-necked flask, add 2.0g of silica microspheres and 150mL of anhydrous toluene, then add 5g of N-(aminoethyl)-?-aminopropyltrimethoxysilane, magnetically stir, 130 o C reflux reaction 20h; Cool to room temperature after completion of the reaction, filter, and the obtained solid is washed 3 times with ethanol, then 50 o C vacuum drying 12h, obtains the silica microspheres of white ethylenediamine modification;

[0064] ②Add 1.5g of ethylenediamine-modified silica microspheres into a 250mL three-neck flask, then add 100mL of water, and add 0.3g of cis-Pt(en)Cl after ultrasonic dispersion 2 , stirring, 40 o C was reacted for 20 h; after the reaction was completed, it was cooled to room temperature, filtered, and the solid was washed 3 times with ethanol, and then dried in vacuo to obtain off-white silica microspheres loaded with divalent plati...

Embodiment 3

[0067] The silica microspheres used in this example are commercially available, with a particle size of 2000 nm.

[0068] ①In a 250mL three-necked flask, add 2.0g of silica microspheres and 150mL of anhydrous toluene, then add 5g of N-(aminoethyl)-?-aminopropyltrimethoxysilane, magnetically stir, 110 o C reflux reaction for 30h; after the completion of the reaction, cool to room temperature, filter, and the resulting solid is washed 3 times with ethanol, and then 50 o C vacuum drying 12h, obtains the silica microspheres of white ethylenediamine modification;

[0069] ②Add 1.5g of ethylenediamine-modified silica microspheres into a 250mL three-neck flask, then add 100mL of water, and add 0.3g of cis-Pt(en)Cl after ultrasonic dispersion 2 , stirring, 40 o C was reacted for 15 hours; after the reaction was completed, it was cooled to room temperature, filtered, and the solid was washed 3 times with ethanol, and then dried in vacuo to obtain off-white silica microspheres loaded ...

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Abstract

The invention discloses reusable load type platinum complex oxidizing agents. The reusable load type platinum complex oxidizing agents are silicon dioxide pellets of load platonic complex, and have a structure shown in a formula (I). In the structure shown in the formula (I), n=3, M is Pt4+, Y is -1 valence halide ions, and grain sizes of the silicon dioxide pellets are 100nanometers to 2,000 nanometers. The invention also provides a preparation method of the oxidizing agents. The preparation method comprises the following steps of (a) using toluene as a solvent and heating the silicon dioxide pellets and a siloxane reagent to perform reflex reaction so as to obtain white solid; (b) performing stirring reaction on the obtained white solid and platinous complex to obtain offwhite solid; and (c) fully reacting the offwhite solid, H2O2 / hydrochloric acid, chlorine or liquid bromine to obtain the load type platinum complex oxidizing agents. The load type platinum complex oxidizing agents are easy to prepare and can be reused after being subjected to regeneration treatment, the yield of synthesized oxidation type polypeptide is not affected by reusing frequency of the oxidizing agents, and the oxidizing agents are recycled and subjected to regeneration treatment simply.

Description

technical field [0001] The invention relates to a loaded oxidant, in particular to a recyclable loaded platinum complex oxidant and its preparation method and application. Background technique [0002] Polypeptide drugs containing intramolecular disulfide bonds have been used in the treatment of various diseases, such as: somatostatin for cancer, calcitonin for Paget's disease, oxytocin for uterine contraction, eptifibatide for antiplatelet, Peptide drugs such as the diabetes treatment drug pramlintide. At present, a large number of polypeptides containing intramolecular disulfide bonds have been developed, which has promoted the development of polypeptide drugs ( Nature Chem. ,2014, 6 ,1009–1016; Eur. J. Med. Chem. ,2014, 77 ,248–257; FutureMed. Chem. ,2009, 1 , 361–377.). The formation of intramolecular disulfide bonds in polypeptide drugs is an important reaction in fine organic chemical and medicinal chemistry. [0003] In the synthesis process of polypeptide d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K1/107C07K5/103C07K7/06C07K7/16
Inventor 霍树营侯晓男刘蒙雨赵晓伟宋常英申世刚
Owner HEBEI UNIVERSITY
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