(NE)-N-(2,2,2-trifluoro-1-phenylethylidene)hydroxylamine

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:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of the above oxime (13.5 g, 71 mmol), 1,2-dibromoethane (65 ml), potassium carbonate (29.4 g, 213 mmol) and acetone (100 ml) was heated at reflux for 16 h and then stirred at room temperature for 7 days. The mixture was filtered and the solvent was evaporated from the filtrate in vacuo to give 20.7 g of 2,2,2-trifluoroacetophenone O-(2-bromoethyl)oxime. was heated at reflux for 16 h The mixture was filtered the solvent was evaporated from the filtrate in vacuo

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

実験手順: A mixture of hydroxylammonium chloride (13.9 g, 200 mmol) and 2,2,2-trifluoroacetophenone (17.4 g, 92 mmol) in absolute ethanol (150 ml) was heated at reflux for 1 h and then stirred at ambient temperature for 16 h. The solvent was evaporated in vacuo, the residue suspended in water (100 ml), filtered and washed with water (20 ml), n-heptane (20 ml) and dried to give 14.0 g 2,2,2-trifluoroacetophenone oxime. was heated at reflux for 1 h The solvent was evaporated in vacuo filtered washed with water (20 ml), n-heptane (20 ml) dried

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

実験手順: A mixture of hydroxylammonium chloride (13.9 g, 200 mmol) and 2,2,2-trifluoroacetophenone (17.4 g, 92 mmol) in absolute ethanol (150 ml) was heated at reflux for 1 h and then stirred at ambient temperature for 16 h. The solvent was evaporated in vacuo, the residue suspended in water (100 ml), filtered and washed with water (20 ml), n-heptane (20 ml) and dried to give 14.0 g 2,2,2-trifluoroacetophenone oxime. was heated at reflux for 1 h The solvent was evaporated in vacuo filtered washed with water (20 ml), n-heptane (20 ml) dried

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: 25 g (0.144 mol) of 2,2,2-Trifluoro-1-phenyl-ethanone are dissolved in 40 ml of ethanol at 80° C. To the solution are added dropwise 10.5 g (0.151 mol) of hydroxylammonium chloride and 20.1 g (0.245 mol) of sodium acetate dissolved in 20 ml of water. The reaction mixture is refluxed overnight, and the solvent is distilled off by a rotary evaporator. The residue is poured into water, the white precipitate is rinsed with water and dried under vacuum, yielding 24.4 g of 2,2,2-trifluoro-1-phenyl-ethanone oxime. The crude product is used in the next step without further purification. The reaction mixture is refluxed overnight the solvent is distilled off by a rotary evaporator The residue is poured into water the white precipitate is rinsed with water dried under vacuum

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

実験手順: 25 g (0.144 mol) of 2,2,2-Trifluoro-1-phenyl-ethanone are dissolved in 40 ml of ethanol at 80° C. To the solution are added dropwise 10.5 g (0.151 mol) of hydroxylammonium chloride and 20.1 g (0.245 mol) of sodium acetate dissolved in 20 ml of water. The reaction mixture is refluxed overnight, and the solvent is distilled off by a rotary evaporator. The residue is poured into water, the white precipitate is rinsed with water and dried under vacuum, yielding 24.4 g of 2,2,2-trifluoro-1-phenyl-ethanone oxime. The crude product is used in the next step without further purification. The reaction mixture is refluxed overnight the solvent is distilled off by a rotary evaporator The residue is poured into water the white precipitate is rinsed with water dried under vacuum

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

実験手順: A mixture of the above oxime (13.5 g, 71 mmol), 1,2-dibromoethane (65 ml), potassium carbonate (29.4 g, 213 mmol) and acetone (100 ml) was heated at reflux for 16 h and then stirred at room temperature for 7 days. The mixture was filtered and the solvent was evaporated from the filtrate in vacuo to give 20.7 g of 2,2,2-trifluoroacetophenone O-(2-bromoethyl)oxime. was heated at reflux for 16 h The mixture was filtered the solvent was evaporated from the filtrate in vacuo

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

実験手順: A mixture of hydroxylammonium chloride (13.9 g, 200 mmol) and 2,2,2-trifluoroacetophenone (17.4 g, 92 mmol) in absolute ethanol (150 ml) was heated at reflux for 1 h and then stirred at ambient temperature for 16 h. The solvent was evaporated in vacuo, the residue suspended in water (100 ml), filtered and washed with water (20 ml), n-heptane (20 ml) and dried to give 14.0 g 2,2,2-trifluoroacetophenone oxime. was heated at reflux for 1 h The solvent was evaporated in vacuo filtered washed with water (20 ml), n-heptane (20 ml) dried