Preparation method of 1-chlorin-4-ethoxy-2,3-difluorobenzene
A technology of ethoxy and difluorobenzene, applied in the field of 1-chloro-4-ethoxy-2
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Embodiment 1
[0010] In a 250ml three-necked flask, add 120ml of chloroform, 50g of 2,3-difluorophenetole, 0.3g of reduced iron powder, start stirring, and lower the temperature. When the temperature drops to -2 degrees Celsius, through the constant pressure dropping funnel Charge 52.3g of chlorine, complete the charge in about 1 hour, keep the reaction temperature at -2 to -8 degrees Celsius, react for 3 hours, and stop the reaction. Add 50ml of aqueous solution (15g of sodium bisulfate dissolved in 50ml of water) to the reaction solution, stir for 0.5h, separate the layers, and wash the lower organic phase with water for 3 to 5 times until neutral. The organic phase was dried with 20 ml of anhydrous sodium sulfate for 2 h, concentrated, and sampled and analyzed to obtain about 75 g of a crude product with a content of 97.1%. Pour 75g of the crude product into a 250ml beaker, recrystallize with petroleum ether, stir, and cool to -2 to -5 degrees Celsius to slowly precipitate crystals. Put...
Embodiment 2
[0012] In a 250ml three-necked flask, add 220ml of chloroform, 80g of 2,3-difluorophenetole, 0.4g of reduced iron powder, start stirring, and lower the temperature. When the temperature drops to -2 degrees Celsius, through the constant pressure dropping funnel Charge 72.3g of chlorine, complete the charge in about 1 hour, keep the reaction temperature at -2 to -5 degrees Celsius, react for 3 hours, and stop the reaction. Add 50ml of aqueous solution (15g of sodium bisulfate dissolved in 50ml of water) to the reaction solution, stir for 0.5h, separate the layers, and wash the lower organic phase with water for 3 to 5 times until neutral. The organic phase was dried with 30 ml of anhydrous sodium sulfate for 2 h, concentrated, and sampled and analyzed to obtain about 97 g of a crude product with a content of 97.1%. Pour 97g of the crude product into a 250ml beaker, recrystallize with petroleum ether, stir, and cool to -2 to -5 degrees Celsius to slowly precipitate crystals. Put...
Embodiment 3
[0014] In a 250ml three-necked flask, add 150ml of chloroform, 60g of 2,3-difluorophenetole, 0.39g of reduced iron powder, start stirring, and lower the temperature. When the temperature drops to -2 degrees Celsius, the Charge 44.9g of chlorine, complete the charge in about 1 hour, keep the reaction temperature at -2 to -8 degrees Celsius, react for 3 hours, and stop the reaction. Add 50ml of aqueous solution (15g of sodium bisulfate dissolved in 50ml of water) to the reaction solution, stir for 0.5h, separate the layers, and wash the lower organic phase with water for 3 to 5 times until neutral. The organic phase was dried with 20 ml of anhydrous sodium sulfate for 2 h, concentrated, and sampled and analyzed to obtain about 69 g of a crude product with a content of 95.1%. Pour 69g of the crude product into a 250ml beaker, recrystallize with petroleum ether, stir, and cool to -2 to -5 degrees Celsius to slowly precipitate crystals. Put it in the refrigerator for 4 hours, and ...
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