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
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[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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