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

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: 2022-04-12
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, product and application of 3-methyl-1,4,2-dioxazol-5-one
  • Preparation method, product and application of 3-methyl-1,4,2-dioxazol-5-one

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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, vacuum distillation was carried out, and the fraction at 89°C / 10mmHg was collected. 109 g of 3-methyl-1,4,2-dioxazol-5-one was obtained 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, 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, and then heated to 110°C. The by-product methanol was fractionated while reacting. After 4 hours of reaction, vacuum distillation was carried out, and the 89°C

[0027] / 10mmHg fraction to obtain 219 g of 3-methyl-1,4,2-dioxazol-5-one with a yield of 82% and a purity of 99.5%.

Embodiment 3

[0029]3-Methyl-1,4,2-dioxazol-5-one, its preparation method is carried out according to the following steps: first, 150 grams of acetohydroxamic acid, 525 grams of dimethyl carbonate and 4 grams of catalyst, wherein containing Dialdehyde 2.7 grams and calcium hydroxide 1.3 grams. Add it into the reaction flask, then heat it to 110°C, fractionate the by-product methanol while reacting, and carry out vacuum distillation after reacting for 4 hours, collect the fraction at 89°C / 10mmHg to obtain 3-methyl-1,4,2 - 164 g of two oxazol-5-ones, the yield is 82%, and the purity is 99.1%.

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Abstract

The invention discloses a preparation method, product and application of 3-methyl-1,4,2-dioxazol-5-ketone, which is characterized in that it is carried out according to the following steps: acetohydroxamic acid, dimethyl carbonate and catalyst into the reaction flask, and then heated to 110°C, and the by-product methanol was fractionated while reacting. After 4 hours of reaction, the reaction liquid was subjected to vacuum distillation, and the fraction at 89°C / 10mmHg was collected to obtain 3-methyl ‑1,4,2‑Dioxazol‑5‑one. The present invention uses the transesterification method to synthesize 3-methyl-1,4,2-dioxazol-5-ketone, with few by-products, and the catalyst can be separated by filtration, which greatly reduces the later purification steps, thereby easily obtaining high-purity products .

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 Patents(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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