4,5-dicyano-2-trifluoromethylimidazole, its preparation intermediate and preparation method of its salt
A technology for trifluoromethyl imidazole salt and trifluoromethyl imidazole, which is applied in the field of chemical synthesis, can solve the problems of low boiling point, volatile measurement, inconvenience of use, etc. , the effect of simple process
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Embodiment 1
[0047] A 1L four-necked round bottom flask equipped with an electric stirrer, reflux condenser, thermometer, and gas tube. Add 43.24g (0.4mol) of diaminomaleonitrile and 51.22g of methyl trifluoroacetate in the glove box at room temperature (0.4mol), 500mL of 1,4-dioxane, set up the device, turn on the ventilation equipment to ensure that there is dry argon protection throughout the reaction. Stir at 25°C for 2h to fully react the two reactants to form amide, and then increase the temperature to the boiling point of 1,4-dioxane (101°C) to ensure the reflux of the system. At this temperature, the amide dehydrates to form imidazole, and stops after refluxing for 2h. The heating reaction is completed, and a mixed solution containing 4,5-dicyano-2-trifluoromethylimidazole is obtained.
[0048] Evaporate the solvent and residual methyl trifluoroacetate under the protection of dry argon, add 600ml of water to the system, add 24g of activated carbon to remove the color, heat a little be...
Embodiment 2
[0051] A 250mL four-necked round bottom flask equipped with an electric stirrer, reflux condenser, thermometer, and gas tube. Add 43.24g (0.4mol) of diaminomaleonitrile and 68.05g of butyl trifluoroacetate in the glove box at room temperature (0.4mol), set up the device, turn on the ventilation equipment to ensure that there is dry argon protection throughout the reaction. Heating to 100°C, the boiling point of butyl trifluoroacetate, facilitates the reflux of the system. At this temperature, the two reactants first generate amide, and then the amide is dehydrated into a ring to form imidazole. The reaction takes 3 hours. After the reaction, the heating is stopped and the reaction system is cooled. A mixed solution containing 4,5-dicyano-2-trifluoromethylimidazole can be obtained.
[0052] Transfer the mixed solution containing 4,5-dicyano-2-trifluoromethylimidazole into a 1L flask, add 600ml of water, add 24g of activated carbon to remove the color, heat it slightly before filte...
Embodiment 3
[0055] A 1L four-necked round bottom flask equipped with an electric stirrer, reflux condenser, thermometer, and gas tube. Add 43.24g (0.4mol) of diaminomaleonitrile and 142.08g of ethyl trifluoroacetate in the glove box at room temperature (1mol), 500mL of 1,4-dioxane, set up the device, turn on the ventilation equipment to ensure that there is dry argon protection throughout the reaction. Stir at 50°C for 2h to fully react the two reactants to form amide, and then increase the temperature to the boiling point of 1,4-dioxane (101°C) to ensure the reflux of the system. At this temperature, the amide dehydrates to form imidazole, and stops after refluxing for 2h. The heating reaction is completed, and a mixed solution containing 4,5-dicyano-2-trifluoromethylimidazole is obtained.
[0056] Evaporate the solvent and residual ethyl trifluoroacetate under the protection of dry argon, add 600ml of water to the system, add 24g of activated carbon to remove the color, heat a little befor...
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