Synthesis method of 3-trifluoromethyl-1, 4, 2-dioxazole-5-one

A technology of trifluoromethyl and synthesis method, applied in the field of battery electrolyte additives, can solve the problems of imperfect manufacturing and purification methods, poor purity, low productivity, etc., and achieves mild reaction process, simple reaction process, and improved yield. Effect

Inactive Publication Date: 2022-01-04

SHIJIAZHUANG SAN TAI CHEM CO LTD +1

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[0003] At present, the production and purification methods of 3-trifluoromethyl-1,4,2-dioxazol-5-one are not perfect enough, and the u...

Abstract

The invention discloses a synthesis method of 3-trifluoromethyl-1, 4, 2-dioxazole-5-one, and relates to the technical field of battery electrolyte additives. The synthesis method comprises the following steps: taking 2, 2, 2-trifluoro-N-hydroxyacetamide and phosgene, and carrying out a cyclization reaction to obtain the 3-trifluoromethyl-1, 4, 2-dioxazole-5-one. Compared with the prior art, the synthesis method of 3-trifluoromethyl-1, 4, 2-dioxazole-5-one has the advantages that the reaction process is milder and safer, the product yield and the product purity in the production process are ensured to be maximized by controlling the reaction conditions in each stage, the product yield is further improved by reasonably controlling the dosage of the reaction raw materials and the reaction process, the yield reaches 54.38% or above, and the purity reaches 99.5% or above.

Application Domain

Organic chemistrySecondary cells servicing/maintenance +1

Technology Topic

TrifluoromethylElectrical battery +9

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Experimental program(6)
Comparison scheme(1)
Effect test(1)

Example Embodiment

[0017] Example 1:

[0018] Synthesis of 3-trifluoromethyl-1,4,2-dioxo-5-one, the following synthesis steps:

[0019] Take the solid 14.84g of phosgene (0.15 mol) was dissolved in 74mL of toluene to give a solution of phosgene in toluene;

[0020] Take 12.9g (0.1mol) -N- hydroxy-2,2,2-trifluoro-acetamide was added to 6.7mL in diethylene glycol dimethyl ether, stirred and dissolved, and then control the temperature of the system 30 ℃, maintaining the temperature of the system 30 deg.] C was slowly added a solution of phosgene in toluene, and then slowly warmed to 60 ℃, maintained 60 ℃, 2,2,2-trifluoro reaction was stirred until the reaction was complete -N- hydroxy-acetamide, heated again to 110 deg.] C the volatiles were evaporated (solvent), and then by fractionating Vigreux fractionating column to give 8.51g of 3-trifluoromethyl-1,4,2-dioxo-5-one, 54.89% yield, 99.6% purity, specific chemical reaction formula as follows:

[0021]

Example Embodiment

[0022] Example 2:

[0023] Synthesis of 3-trifluoromethyl-1,4,2-dioxo-5-one, the following steps synthesis

[0024] Take the solid 16.82g of phosgene (0.17 mol) was dissolved in 84mL of toluene to give a solution of phosgene in toluene;

[0025] Take 12.9g (0.1mol) -N- hydroxy-2,2,2-trifluoro-acetamide was added to 6.9mL in diethylene glycol dimethyl ether, stirred and dissolved, and then control the temperature of the system is 25 ℃, maintaining the temperature of the system 25 deg.] C was slowly added a solution of phosgene in toluene, and then slowly warmed to 70 ℃, maintained 70 ℃, 2,2,2-trifluoro reaction was stirred until the reaction was complete -N- hydroxy-acetamide, heated again to 118 ℃ volatiles were evaporated (solvent), and then by fractionating Vigreux fractionating column to give 8.72g of 3-trifluoromethyl-1,4,2-dioxo-5-one, 56.25% yield, 99.5% purity.

Example Embodiment

[0026] Example 3:

[0027] Synthesis of 3-trifluoromethyl-1,4,2-dioxo-5-one, the following synthesis steps:

[0028] Take the solid 13.85g of phosgene (0.14 mol) was dissolved in 84mL of toluene to give a solution of phosgene in toluene;

[0029] Take 12.9g (0.1mol) -N- hydroxy-2,2,2-trifluoro-acetamide was added to 6.5mL in diethylene glycol dimethyl ether, stirred and dissolved, and then control the temperature of the system is 20 ℃, maintaining the temperature of the system 20 ℃ toluene solution was slowly added phosgene and then slowly warmed to 65 ℃, maintained 65 ℃, 2,2,2-trifluoro reaction was stirred until the reaction was complete -N- hydroxy-acetamide, heated again to 115 deg.] C the volatiles were evaporated (solvent), and then by fractionating Vigreux fractionating column to give 8.43g of 3-trifluoromethyl-1,4,2-dioxo-5-one, 54.38% yield, 99.7% purity.

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Classification and recommendation of technical efficacy words

The reaction process is simple
mild reaction process

Synthesis method of 3-trifluoromethyl-1, 4, 2-dioxazole-5-one

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Problems solved by technology

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Description & Claims & Application Information

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