2-bromo-1-(2,3-dichlorophenyl)ethanone

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: At RT, 411 mg (4.33 mmol) of sodium diformylamide were added to 1.0 g (3.73 mmol) of 2-bromo-1-(2,3-dichlorophenyl)ethanone [for the preparation, see for example U.S. Pat. No. 5,831,132] in 4 ml of acetonitrile, and the mixture was stirred at RT overnight. The mixture was then heated to 70° C. and filtered whilst still warm. The solid that remained was washed with 2 ml of hot acetonitrile. The combined filtrates were freed from the solvent on a rotary evaporator. 10 ml of a 5% strength ethanolic hydrogen chloride solution were added to the dark-brown oily residue, and the mixture was stirred at RT overnight. The volatile components were removed on a rotary evaporator and the yellow solid that remained was stirred in 20 ml of boiling diethyl ether. After cooling to RT, the solid was isolated by filtration, washed with diethyl ether and dried under high vacuum. This gave 410 mg (46% of theory) of the title compound. for the preparation filtered whilst still warm The solid that remained was washed with 2 ml of hot acetonitrile The combined filtrates were freed from the solvent on a rotary evaporator 10 ml of a 5% strength ethanolic hydrogen chloride solution were added to the dark-brown oily residue The volatile components were removed on a rotary evaporator the yellow solid that remained was stirred in 20 ml of boiling diethyl ether After cooling to RT the solid was isolated by filtration washed with diethyl ether dried under high vacuum

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

実験手順: A solution of 2-bromo-1-(2,3-dichlorophenyl)ethanone (4.25 g, 15.9 mmol) and potassium thiocyanate (1.54 g, 15.9 mmol) in ethanol (40 ml) was stirred at 80° C. for 2 hours. After cooling to room temperature, water (70 ml) was poured to the reaction mixture, and crystals were collected by filtration and washed with water to give 3.10 g (79.5%) of the desired product as a solid. were collected by filtration washed with water

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

実験手順: Bromine (2.54 g, 15.9 mmol) was slowly added dropwise to a solution of 1-(2,3-dichlorophenyl)ethanone (3.00 g, 15.9 mmol) in diethyl ether (60 ml), and the mixture was stirred at room temperature for 4 hours. The reaction mixture was distilled off under reduced pressure to give 2-bromo-1-(2,3-dichlorophenyl)ethanone as an oil quantitatively. The reaction mixture was distilled off under reduced pressure

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

実験手順: Bromine (2.54 g, 15.9 mmol) was slowly added dropwise to a solution of 1-(2,3-dichlorophenyl)ethanone (3.00 g, 15.9 mmol) in diethyl ether (60 ml), and the mixture was stirred at room temperature for 4 hours. The reaction mixture was distilled off under reduced pressure to give 2-bromo-1-(2,3-dichlorophenyl)ethanone as an oil quantitatively. The reaction mixture was distilled off under reduced pressure

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: At RT, 411 mg (4.33 mmol) of sodium diformylamide were added to 1.0 g (3.73 mmol) of 2-bromo-1-(2,3-dichlorophenyl)ethanone [for the preparation, see for example U.S. Pat. No. 5,831,132] in 4 ml of acetonitrile, and the mixture was stirred at RT overnight. The mixture was then heated to 70° C. and filtered whilst still warm. The solid that remained was washed with 2 ml of hot acetonitrile. The combined filtrates were freed from the solvent on a rotary evaporator. 10 ml of a 5% strength ethanolic hydrogen chloride solution were added to the dark-brown oily residue, and the mixture was stirred at RT overnight. The volatile components were removed on a rotary evaporator and the yellow solid that remained was stirred in 20 ml of boiling diethyl ether. After cooling to RT, the solid was isolated by filtration, washed with diethyl ether and dried under high vacuum. This gave 410 mg (46% of theory) of the title compound. for the preparation filtered whilst still warm The solid that remained was washed with 2 ml of hot acetonitrile The combined filtrates were freed from the solvent on a rotary evaporator 10 ml of a 5% strength ethanolic hydrogen chloride solution were added to the dark-brown oily residue The volatile components were removed on a rotary evaporator the yellow solid that remained was stirred in 20 ml of boiling diethyl ether After cooling to RT the solid was isolated by filtration washed with diethyl ether dried under high vacuum