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

Method used

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

Examples

Experimental program
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Example Embodiment

[0018] Example 1:

[0019] Synthesis of pentafluorophenyl dioxyloxazolone, its synthetic steps are as follows:

[0020] 36.79 g (0.162 mol) of 2,3,4,5,6-pentafluoro-N-hydroxy-benzamide was dissolved in 400 mL of fresh steamed dichloromethane, and then 16.2 g (0.1 mol) N, N '- carbonyl dimimidazole, room temperature for 15 min, TLC monitors to N, N'-carbonyl diimidazole reaction, adding 810 ml of concentration of 1 mol / L, aqueous hydrochloric acid aqueous hydrochloric acid is mixed, and then adding 500 ml of ethyl acetate extraction. , Phase phase, ethyl acetate is packed with anhydrous magnesium sulfate, concentrated under reduced pressure, and 8.79 g of 3- (2, 3, 4, 5, 6-phenyl) -1, 4, 2-two The oxypole-5-ketone, yield of 33.41%, purity 99.6%, and the specific chemical reaction formula is as follows:

Example Embodiment

[0021] Example 2:

[0022] Synthetic method of pentafluorophenyl dioxyphenolidone, the synthesis steps are as follows

[0023] 34.06 g (0.15 mol) of 2,3,4,5,6-pentafluoro-N-hydroxy-benzamide was dissolved in 324 ml of fresh steamed dichloromethane, and then 16.2 g (0.1 mol) N, N '- carbonyl dimimidazole, room temperature for 30 min, TLC monitors to N, N'-carbonyl diimidazole reaction, adding 405 ml of concentration of 2 mol / L, aqueous hydrochloric acid aqueous hydrochloric acid is mixed, and then add 400 ml of ethyl acetate extraction. , Phase phase, ethyl acetate phase is phased with anhydrous magnesium sulfate, concentrated under reduced pressure, and 8.81 g of 3- (2, 3, 4, 5, 6-phenyl) -1, 4, 2- 2 The oxypole-5-ketone has a yield of 33.49%, and the purity is 99.5%.

Example Embodiment

[0024] Example 3:

[0025] Synthesis of pentafluorophenyl dioxyloxazolone, its synthetic steps are as follows:

[0026] 40.88 g (0.18 mol) of 2,3,4,5,6-pentafluoro-N-hydroxy-benzamide was dissolved in 390 ml of fresh steamed dichloromethane, and then 16.2 g (0.1 mol) N, N, N '- carbonyl dimimidazole, room temperature for 10 min, TLC monitors to N, N'-carbonyl diimidazole reaction, adding 650 ml of concentration of 1.5 mol / L, aqueous hydrochloric acid aqueous hydrochloric acid is stirred, and then adding 500 ml of ethyl acetate EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc (EtOAc) Dioxazole-5-ketone, yield of 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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