Synthetic method for 2,4-difluorobiphenyl
A technology of difluorobiphenyl and synthesis method, which is applied in the field of synthesis of 2,4-difluorobiphenyl and 2,4-difluorobiphenyl, and can solve the problems of lengthy reaction steps, low yield, complicated operation, etc. To achieve the effect of short process, simple reaction process and avoid high temperature reaction
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Embodiment 1
[0019] Add 114g (1mol) of trifluoroacetic acid (1mol), 5.7g of anhydrous magnesium sulfate, 1.3g of catalyst and 134ml of benzene (1.5mol) into the reaction kettle, stir and cool to 2°C, add 128.9g (1.1mol) of isoamyl nitrite, Control the temperature at 6°C, add 130.1g (1mol) of 2,4-difluoroaniline dropwise therein, control the reaction temperature at 10°C during the dropwise addition process, stir and react at 5°C for 1h after the addition, and put the reaction The mixture was filtered with suction, washed with benzene three times, then washed with water until neutral, dried and distilled under reduced pressure to obtain a light yellow solid.
[0020] Decolorize the obtained light yellow solid with activated carbon, add 3 times the weight of ethanol, stir at room temperature for 20 minutes, decarburize and filter, put the filtrate into the crystallization kettle, and when the temperature of the crystallization kettle drops to 10°C, discharge the material for solid-liquid separ...
Embodiment 2
[0023] Add 34.2g (0.3mol) of trifluoroacetic acid, 10.26g of anhydrous magnesium sulfate, 0.52g of catalyst and 35.5ml of benzene (0.4mol) into the reaction kettle, stir and cool to 3°C, add 35.2g (0.3mol) of isoamyl nitrite mol), the temperature was controlled at 7°C, 26.02g (0.2mol) of 2,4-difluoroaniline was added dropwise therein, the reaction temperature was controlled to be 15°C during the dropwise addition, and the reaction was stirred at 7°C for 1.5h after the addition was completed. After the reaction, the reaction mixture was suction filtered, washed with benzene three times, then washed with water until neutral, dried, and distilled under reduced pressure to obtain a light yellow solid.
[0024] Decolorize the obtained light yellow solid with activated carbon, add 3 times the weight of ethanol, stir at room temperature for 25 minutes, decarburize and filter, and put the filtrate into the crystallization kettle. When the temperature of the crystallization kettle drops...
Embodiment 3
[0027] Add 68.4g (0.6mol) of trifluoroacetic acid, 13.68g of anhydrous magnesium sulfate, 0.98g of catalyst and 71ml of benzene (0.8mol) into the reaction kettle, stir and cool to 4°C, add 70.4g (0.6mol) of isoamyl nitrite ), control the temperature at 8°C, add 65.05g (0.5mol) of 2,4-difluoroaniline dropwise therein, control the reaction temperature at 17°C during the dropwise addition process, stir and react at 9°C for 2h after the addition, and the reaction ends Afterwards, the reaction mixture was suction filtered, washed with benzene three times, and then washed with water until neutral, dried, and distilled under reduced pressure to obtain a light yellow solid.
[0028] Decolorize the obtained light yellow solid with activated carbon, add 3 times the weight of ethanol, stir at room temperature for 30 minutes, decarburize and filter, and put the filtrate into the crystallization kettle. When the temperature of the crystallization kettle drops to 10°C, discharge the material...
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