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Macromolecule-loaded oxidizing agent containing iodine with high valence, and preparation method and application thereof

A high-valence iodine and high-molecular loading technology, applied in the field of oxidants, achieves the effects of mild reaction conditions, broad application prospects, and convenient post-processing

Pending Publication Date: 2020-05-08
PANASIA OLAUGHLIN BIO TECH WUHAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the production cost and use safety problems of iodine-containing oxidants in the prior art, to provide a kind of oxidant containing high valence iodine loaded with high valence iodine, which is easy to prepare and low in cost, as well as its preparation method and use, so as to obtain high Molecularly loaded oxidants containing high valence iodine have good stability and have little impact on the environment

Method used

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  • Macromolecule-loaded oxidizing agent containing iodine with high valence, and preparation method and application thereof
  • Macromolecule-loaded oxidizing agent containing iodine with high valence, and preparation method and application thereof
  • Macromolecule-loaded oxidizing agent containing iodine with high valence, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0021] Add 600 ml of N,N-dimethylformamide and 150 g of chloromethyl polystyrene resin (1% DVB cross-linked, 100–200 mesh, 1.1 mmol / g) into a reaction flask equipped with a mechanical stirrer, Stir at room temperature for 2 hours; then add 61.4 gram of 2-iodobenzoic acid (molecular weight is 248), 13.8 gram of potassium hydroxide powder (molecular weight is 56) and 3.76 gram cesium fluoride (molecular weight is 152); Stir at room temperature for 30 minutes, Then stirred at 60-80 degrees for 5 hours; filtered after cooling to room temperature, the resin was successively washed with 200 ml of water, 200 ml of methanol, 200 ml of methylene chloride, 200 ml of methanol, 200 ml of methylene chloride, and 200 ml of dichloromethane. Washed with 1 ml of methanol; after vacuum drying overnight, 179.8 g of 2-iodobenzoic acid substituted resin was obtained.

[0022] Add 363 ml of N,N-dimethylformamide, 24 grams of potassium monopersulfate (Oxone) into a reaction flask equipped with a mec...

Embodiment 2

[0024] The polymer loaded oxidant containing high valence iodine prepared in the present invention is mainly used for the oxidation of alcohols, and the reaction formula between the polymer loaded oxidant containing high valence iodine and alcohol oxidation is as follows figure 2 shown. Specifically, in this embodiment, 50 ml of methylene chloride, 10 g of polymer-loaded oxidant resin and 0.8 g of benzyl alcohol were added to a reaction flask equipped with a mechanical stirrer, and stirred at room temperature for 30 minutes; gas chromatography monitored , benzyl alcohol was completely converted into benzaldehyde; filtered, the filtered resin was washed with 10 ml of dichloromethane, and the combined supernatant was concentrated to obtain 0.76 g of benzaldehyde with a purity of >98%.

Embodiment 3

[0026] The polymer loaded oxidant containing high valence iodine prepared in the present invention is mainly used for the oxidation of alcohols, and the reaction formula between the polymer loaded oxidant containing high valence iodine and alcohol oxidation is as follows figure 2 shown. Specifically, in this embodiment, 50 ml of dichloromethane, 10 g of polymer-loaded oxidant resin and 1.1 g of citronellol (molecular weight: 156) were added to a reaction flask equipped with a mechanical stirrer, and stirred at room temperature for 30 Minutes; gas chromatography monitoring, citronellol is completely converted into citronellal; filter, the filtered resin is washed with 10 ml of dichloromethane, and the combined supernatant is concentrated to obtain 0.98 g of citronellal, with a purity of >98%.

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Abstract

The invention discloses a macromolecule-loaded oxidizing agent containing iodine with high valence, and a preparation method and an application thereof. 2-iodobenzoic acid is used as a raw material and is loaded on chloromethyl polystyrene resin under an alkaline condition, and iodine is oxidized into high valence by using potassium monopersulfate. The macromolecule-loaded oxidizing agent containing iodine with high valence, prepared through the method can oxidize primary alcohol into aldehyde and, secondary alcohol into ketone, and a reaction byproduct is water; the reaction conditions are mild, the post-treatment is convenient, and the macromolecular-loaded oxidizing agent containing iodine with high valence can be separated from the reaction system only by simple filtration; and the macromolecule-loaded oxidizing agent containing iodine with high valence can be recycled for multiple times, so that the influence on the environment and the production cost are reduced. Besides, the macromolecular-loaded oxidizing agent containing iodine with high valence is simple and convenient to prepare, effectively solves the problems of stability and high cost of a micromolecular iodine-containing oxidizing agent, and has a wide application prospect in the field of fine chemical engineering.

Description

technical field [0001] The invention relates to the technical field of oxidants, in particular to an oxidant loaded with high valence iodine, a preparation method and application thereof. Background technique [0002] Oxidation reactions play an important role in organic chemistry and are widely used in the pharmaceutical industry and fine chemical industry. In recent years, common oxidants such as high valence compounds of metal elements such as potassium permanganate, manganese dioxide, potassium dichromate, chromic acid and lead tetraacetate have received more and more attention because of their environmental pollution and difficult handling. limits. The application of green oxidants such as hydrogen peroxide, air, and oxygen is gradually increasing. However, many oxidation reactions do not work well with hydrogen peroxide, air, or oxygen. It is still an important direction in the research of organic chemistry to continue to seek green and environmentally friendly oxid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/30C07C47/54C07C47/21C07C49/78
CPCC07C45/30C07C47/54C07C47/21C07C49/78
Inventor 陈臻
Owner PANASIA OLAUGHLIN BIO TECH WUHAN CO LTD
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