Preparation method of 3-methyl-1, 4, 2-dioxazole-5-one, product and application

A technology of dioxazole and methyl, applied in 3-methyl-1,4,2-dioxazol-5-one, 3-methyl-1,4,2-dioxazol-5-one In the field of preparation, it can solve the problems of less disclosure, achieve the effect of less by-products and reduce the purification steps in the later stage

Active Publication Date: 2020-09-22
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above scheme only discloses dioxazolone electrolyte additives with electron-withdrawing groups, and the dioxazolone electrolyte additives with electron-donating groups are less disclosed in this technical scheme and prior art materials

Method used

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  • Preparation method of 3-methyl-1, 4, 2-dioxazole-5-one, product and application
  • Preparation method of 3-methyl-1, 4, 2-dioxazole-5-one, product and application

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 3-Methyl-1,4,2-dioxazol-5-one, its preparation method is carried out according to the following steps: first, 100 grams of acetohydroxamic acid, 240 grams of dimethyl carbonate and 2.4 grams of catalyst, wherein containing 1.59 grams of dialdehyde and 0.81 grams of calcium hydroxide were added to the reaction flask, then heated to 110°C, and the by-product methanol was fractionated while reacting. After 4 hours of reaction, the reaction solution was distilled under reduced pressure and collected at 89°C / 109 g of 3-methyl-1,4,2-dioxazol-5-one was obtained in a fraction of 10 mmHg, with a yield of 81% and a purity of 99.7%.

Embodiment 2

[0026] 3-Methyl-1,4,2-dioxazol-5-one, its preparation method is carried out according to the following steps: first, 200 grams of acetohydroxamic acid, 720 grams of dimethyl carbonate and 10 grams of catalyst, wherein containing ethyl 5.2 grams of dialdehyde and 6 grams of barium hydroxide were added to the reaction flask, then heated to 110°C, and the by-product methanol was fractionated while reacting. After 4 hours of reaction, the reaction solution was distilled under reduced pressure and collected at 89°C / 227 g of 3-methyl-1,4,2-dioxazol-5-one was obtained in a fraction of 10 mmHg, with a yield of 85% and a purity of 99.2%.

Embodiment 3

[0028]3-Methyl-1,4,2-dioxazol-5-one, its preparation method is carried out according to the following steps: first, 200 grams of acetohydroxamic acid, 700 grams of dimethyl carbonate and 6 grams of catalyst, wherein containing 4 grams of dialdehyde and 2 grams of calcium hydroxide were added to the reaction flask, then heated to 110°C, and the by-product methanol was fractionated while reacting. After 4 hours of reaction, the reaction solution was distilled under reduced pressure and collected at 89°C / 10 mmHg fraction, 219 g of 3-methyl-1,4,2-dioxazol-5-one was obtained, with a yield of 82% and a purity of 99.5%.

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Abstract

The invention discloses a preparation method of 3-methyl-1, 4, 2-dioxazole-5-one, a product and application. The method is characterized by comprising the following steps of: adding acetohydroxamic acid, dimethyl carbonate and a catalyst into a reaction flask, performing heating to 110DEG C, carrying out reaction while fractionating a byproduct methanol, carrying out the reaction for 4h, then carrying out reduced pressure distillation on the reaction liquid, and collecting 89DEG C/10mmHg fraction to obtain 3-methyl-1, 4, 2-dioxazole-5-one. According to the method, the 3-methyl-1, 4, 2-dioxazole-5-one is synthesized by using an ester exchange method, few byproducts are produced, the catalyst can be separated after being filtered, and the later purification step is greatly reduced, so that ahigh-purity product is easy to obtain.

Description

technical field [0001] The invention belongs to the technical field of electrolyte additives for rechargeable lithium-ion battery systems, and in particular relates to a preparation method of 3-methyl-1,4,2-dioxazol-5-one and 3-methanol prepared by the method. Base-1,4,2-dioxazol-5-one and its application. Background technique [0002] In recent years, my country's new energy industry has developed rapidly, especially electric vehicles represented by power lithium-ion batteries. However, power lithium-ion batteries have problems such as long charging time and short cruising range. To break through the above problems, developing a new type of additive is a cost-effective strategy. [0003] Chinese patent application, application number CN201810377636.6, application date 2018.04.25, application publication number CN110400968A, application publication date 2019.11.01, discloses a non-aqueous electrolyte, a power battery containing the non-aqueous electrolyte, and a power batte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D273/01H01M10/0525H01M10/0567
CPCC07D273/01H01M10/0567H01M10/0525H01M2300/0025Y02E60/10
Inventor 吴国栋沈鸣曹娜周立新
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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