trifluoromethoxybenzene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:120.01; pressure:0.00; stir:

反応条件: temp:120.01; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 250 ml stainless steel reactor equipped with a magnetic stirrer system, 100 ml of anhydrous HF, 23.6 g (0.3 mole) of acetyl chloride, and 32.4 g (0.2 mole) of trifluoromethoxybenzene were introduced at around 0° C. The reactor was closed and gaseous boron trifluoride (BF3) introduced until a constant pressure of 6 bars was achieved. The reaction was then allowed to proceed with stirring at ambient temperature for 3 hours. Following reaction, the reactor was decompressed to atmospheric pressure, then the reaction mixture poured over 200 g of crushed ice. The resultant heterogeneous mixture was extracted three times with 200 ml of methylene chloride. The organic phases were washed three times with 200 ml of water, once with 200 ml of 3% aqueous potassium hydroxide solution, and twice with 200 ml of water. The organic phase was dried over magnesium sulfate and the solvent eliminated by distillation under reduced pressure. 37.2 g (yield: 91%) of p-trifluoromethoxyacetophenone having a purity of 96.3% was recovered. were introduced at around 0° C The reactor was closed reaction The resultant heterogeneous mixture was extracted three times with 200 ml of methylene chloride The organic phases were washed three times with 200 ml of water The organic phase was dried over magnesium sulfate the solvent eliminated by distillation under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 250 ml stainless steel reactor equipped with a magnetic stirrer system, 100 ml of anhydrous HF, 23.6 g (0.3 mole) of acetyl chloride, and 32.4 g (0.2 mole) of trifluoromethoxybenzene were introduced at around 0° C. The reactor was closed and gaseous boron trifluoride (BF3) introduced until a constant pressure of 6 bars was achieved. The reaction was then allowed to proceed with stirring at ambient temperature for 3 hours. Following reaction, the reactor was decompressed to atmospheric pressure, then the reaction mixture poured over 200 g of crushed ice. The resultant heterogeneous mixture was extracted three times with 200 ml of methylene chloride. The organic phases were washed three times with 200 ml of water, once with 200 ml of 3% aqueous potassium hydroxide solution, and twice with 200 ml of water. The organic phase was dried over magnesium sulfate and the solvent eliminated by distillation under reduced pressure. 37.2 g (yield: 91%) of p-trifluoromethoxyacetophenone having a purity of 96.3% was recovered. were introduced at around 0° C The reactor was closed reaction The resultant heterogeneous mixture was extracted three times with 200 ml of methylene chloride The organic phases were washed three times with 200 ml of water The organic phase was dried over magnesium sulfate the solvent eliminated by distillation under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 100 mL flask equipped with a stir-bar and a nitrogen bubbler was charged with (trifluoromethoxy)-benzene (5.015 g) at room temperature. Oleum (15% SO3, 9.30 g) was added to the above flask at 10° C. The reaction mixture was allowed to warm to room temperature and stirred at room temperature for 15 h. A sodium hydroxide solution (7.75 g, in 23 mL water) was slowly added to the reaction mixture while the reaction mixture was cooled with an ice-water bath. The resulting solid was collected by filtration, dried under vacuum, and then extracted with refluxing ethanol. The ethanol solution was dried to give sodium 4-(trifluoromethoxy)benzenesulfonate (3FMBSNa) 2.0 g (yield 24%): 1H NMR (D2O) 7.45 (d, J=9 Hz, 2H), 7.89 (m, 2H) ppm; 19F NMR (D2O)-58.1 (s) ppm. A 100 mL flask equipped with a stir-bar was cooled with an ice-water bath The resulting solid was collected by filtration dried under vacuum extracted with refluxing ethanol The ethanol solution was dried

反応条件: temp:0.00; pressure:0.00; stir: