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Synthesis method of pentafluorophenyl dioxazolone

A technology of pentafluorophenyl azlactone and its synthesis method, which is applied in the field of synthesis of pentafluorophenyl azlactone, and can solve problems such as poor purity, low production capacity, and imperfect pentafluorophenyl azlactone , to achieve the effect of simple reaction process, mild reaction process and improved yield

Inactive Publication Date: 2021-12-21
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production and purification methods of pentafluorophenyldioxazolone are not perfect enough, and the uncertainty of various parameters in the manufacturing process leads to low production capacity and relatively poor purity

Method used

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  • Synthesis method of pentafluorophenyl dioxazolone
  • Synthesis method of pentafluorophenyl dioxazolone
  • Synthesis method of pentafluorophenyl dioxazolone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The synthetic method of pentafluorophenyl dioxazolone, its synthetic steps are as follows:

[0020] Take 36.79g (0.162mol) of 2,3,4,5,6-pentafluoro-N-hydroxyl-benzamide and dissolve it in 400mL of freshly distilled dichloromethane, then add 16.2g (0.1mol) of N,N '-Carbonyldiimidazole, carry out cyclization reaction at room temperature for 15min, TLC monitors until the reaction of N,N'-carbonyldiimidazole is complete, add 810mL of 1mol / L hydrochloric acid aqueous solution and stir for neutralization reaction, then add 500mL of ethyl acetate to extract , phase separation, the resulting ethyl acetate phase was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 8.79 g of 3-(2,3,4,5,6-pentafluorophenyl)-1,4,2-bis Oxazol-5-one, yield 33.41%, purity 99.6%, specific chemical reaction formula is as follows:

Embodiment 2

[0022] The synthetic method of pentafluorophenyl dioxazolone, its synthetic steps are as follows

[0023] Take 34.06g (0.15mol) of 2,3,4,5,6-pentafluoro-N-hydroxy-benzamide and dissolve it in 324mL of freshly distilled dichloromethane, then add 16.2g (0.1mol) of N,N '-Carbonyldiimidazole, carry out cyclization reaction at room temperature for 30min, TLC monitors until the reaction of N,N'-carbonyldiimidazole is complete, add 405mL aqueous hydrochloric acid solution with a concentration of 2mol / L and stir for neutralization reaction, then add 400mL ethyl acetate to extract , phase separation, the resulting ethyl acetate phase was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 8.81 g of 3-(2,3,4,5,6-pentafluorophenyl)-1,4,2-bis Oxazol-5-one, yield 33.49%, purity 99.5%.

Embodiment 3

[0025] The synthetic method of pentafluorophenyl dioxazolone, its synthetic steps are as follows:

[0026] Take 40.88g (0.18mol) of 2,3,4,5,6-pentafluoro-N-hydroxyl-benzamide and dissolve it in 390mL of freshly distilled dichloromethane, then add 16.2g (0.1mol) of N,N '-Carbonyldiimidazole, carry out cyclization reaction at room temperature for 10min, TLC monitors until the reaction of N,N'-carbonyldiimidazole is complete, add 650mL of 1.5mol / L hydrochloric acid aqueous solution and stir for neutralization reaction, then add 500mL of ethyl acetate Extraction and phase separation, the resulting ethyl acetate phase was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 8.62 g of 3-(2,3,4,5,6-pentafluorophenyl)-1,4,2- Dioxazol-5-one, yield 32.77%, purity 99.6%.

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Abstract

The invention discloses a synthesis method of pentafluorophenyl dioxazolone, and relates to the technical field of battery electrolytic solution additives. The synthesis method comprises the following steps: taking 2, 3, 4, 5, 6-pentafluoro-N-hydroxy-benzamide and N, N'-carbonyl diimidazole, and carrying out a cyclization reaction to obtain the pentafluorophenyl dioxazolone. Compared with the prior art, the synthesis method of pentafluorophenyl dioxazolone has the advantages that the reaction process is milder and safer, the product yield and the product purity in the production process are maximized by controlling the reaction conditions in each stage, the product yield is further improved by reasonably controlling the use amount of the reaction raw materials and the reaction process, the yield reaches 32.61% or above and the purity reaches 99.5% or above.

Description

technical field [0001] The invention relates to the technical field of battery electrolyte additives, in particular to a synthesis method of pentafluorophenyldioxazolone. Background technique [0002] Lithium-ion batteries are currently the most common electrical energy storage devices. Compared with traditional batteries, they have higher storage capacity and more stable performance. The key factor affecting the performance of lithium-ion batteries lies in the performance of organic electrolytes. In battery production In the electrolyte, an electrolyte additive containing pentafluorophenyldioxazolone is added to increase the concentration of hydrogen ions in the electrolyte so as to reduce the loss in the process of electric energy conversion. [0003] At present, the production and purification methods of pentafluorophenyldioxazolone are not perfect enough, and the uncertainty of various parameters in the production process leads to low production capacity and relatively p...

Claims

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Application Information

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IPC IPC(8): C07D273/01H01M10/0525H01M10/0567
CPCC07D273/01H01M10/0567H01M10/0525Y02E60/10
Inventor 闫朋飞杨世雄赵光华高山林胜赛李庆占邢艳召刘鹏田丽霞张茜张民彭鹏鹏郝俊侯荣雪王军葛建民武利斌闫彩桥许晓丹
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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