P-chlorobenzotrifluoride clean nitration reaction catalyzed by heteropoly acid ionic liquid
A technology of p-chlorotrifluorotoluene and ionic liquid, which can be used in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry and other directions, and can solve the problems of difficult separation and purification, environmental hazards and high cost , to achieve the effect of wide source of raw materials, high catalytic activity and convenient preparation
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Embodiment 1
[0022] In a 25mL round bottom flask, add 10mmol (1.81g) p-chlorobenzotrifluoride, 30mmol (2.8g) 65% nitric acid, 1.0mmol catalyst (the anion is H 2 PMo 12 o 40 - ), mixed and stirred for 10 hours at 80° C., cooled, and allowed to stand for phase separation. The crude product in the upper layer was washed with water, neutralized, and vacuum-dried to obtain the pure product 4-chloro-3-nitrobenzotrifluoride, with a yield of 80%.
Embodiment 2
[0024] In a 25mL round bottom flask, add 10mmol (1.81g) p-chlorobenzotrifluoride, 20mmol (1.26g) 100% nitric acid, 0.5mmol catalyst (the anion is H 2 PMo 12 o 40 - ), mixed and stirred for 1 hour at 20° C., cooled, and allowed to stand for phase separation. The crude product in the upper layer was washed with water, neutralized, and vacuum-dried to obtain the pure product 4-chloro-3-nitrobenzotrifluoride, with a yield of 83%.
Embodiment 3
[0026] In a 25mL round bottom flask, add 10mmol (1.81g) p-chlorobenzotrifluoride, 10mmol (0.63g) 100% nitric acid, 0.5mmol catalyst (the anion is H 2 PMo 12 o 40 - ), mixed and stirred for 5 hours at 50° C., cooled, left to stand for phase separation, and the crude product in the upper layer was washed with water, neutralized and dried in vacuo to obtain the pure product 4-chloro-3-nitrobenzotrifluoride, with a yield of 95%.
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