1-(2,4-difluorophenyl)-2-fluoroethanone

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

実験手順: A solution of 2,2',4'-trifluoroacetophenone (1.60 g; 9.2 mM) in sulphuryl chloride (4 ml) was heated at 75° for 18 hours. The mixture was then cooled and iced-water (40 ml) was added. The product was extracted into ether (80 ml), which was washed with water and aqueous sodium bicarbonate solution, and then dried over magnesium sulphate. Evaporation yielded the desired product as a colourless, intensely lachrymatory liquid (2.0 g; 100%). The mixture was then cooled The product was extracted into ether (80 ml), which was washed with water and aqueous sodium bicarbonate solution dried over magnesium sulphate Evaporation

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

実験手順: 1,3-Difluorobenzene (2.02 g; 17.7 mM) and anhydrous aluminium chloride (2.60 g; 19.47 mM) were stirred together under dry nitrogen at room temperature. A solution of fluoroacetyl chloride (1,71 g; 17.7 mM) in anhydrous methylene chloride (2 ml) was added over 30 minutes. The mixture was then warmed at about 50° for 3 hours. On cooling methylene chloride (40 ml) was added and the mixture was poured onto ice. The methylene chloride layer was separated, dried over magnesium sulphate and evaporated to give a white solid. This material was chromatographed on a column of silica eluting with a mixture of hexane/methylene chloride (65:35 by volume). The product-containing fractions were collected. The title compound crystallised on evaporation of these fractions and was dried in a vacuum desiccator to a colourless crystalline solid (1.12 g; 36% yield), melting point 57°-8°. The mixture was then warmed at about 50° for 3 hours was added the mixture was poured onto ice The methylene chloride layer was separated dried over magnesium sulphate evaporated to give a white solid This material was chromatographed on a column of silica eluting with a mixture of hexane/methylene chloride (65:35 by volume) The product-containing fractions were collected The title compound crystallised on evaporation of these fractions was dried in a vacuum desiccator to a colourless crystalline solid (1.12 g; 36% yield), melting point 57°-8°

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

実験手順: 1,3-Difluorobenzene (2.02 g; 17.7 mM) and anhydrous aluminium chloride (2.60 g; 19.47 mM) were stirred together under dry nitrogen at room temperature. A solution of fluoroacetyl chloride (1,71 g; 17.7 mM) in anhydrous methylene chloride (2 ml) was added over 30 minutes. The mixture was then warmed at about 50° for 3 hours. On cooling methylene chloride (40 ml) was added and the mixture was poured onto ice. The methylene chloride layer was separated, dried over magnesium sulphate and evaporated to give a white solid. This material was chromatographed on a column of silica eluting with a mixture of hexane/methylene chloride (65:35 by volume). The product-containing fractions were collected. The title compound crystallised on evaporation of these fractions and was dried in a vacuum desiccator to a colourless crystalline solid (1.12 g; 36% yield), melting point 57°-8°. The mixture was then warmed at about 50° for 3 hours was added the mixture was poured onto ice The methylene chloride layer was separated dried over magnesium sulphate evaporated to give a white solid This material was chromatographed on a column of silica eluting with a mixture of hexane/methylene chloride (65:35 by volume) The product-containing fractions were collected The title compound crystallised on evaporation of these fractions was dried in a vacuum desiccator to a colourless crystalline solid (1.12 g; 36% yield), melting point 57°-8°

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

実験手順: A solution of 2,2',4'-trifluoroacetophenone (1.60 g; 9.2 mM) in sulphuryl chloride (4 ml) was heated at 75° for 18 hours. The mixture was then cooled and iced-water (40 ml) was added. The product was extracted into ether (80 ml), which was washed with water and aqueous sodium bicarbonate solution, and then dried over magnesium sulphate. Evaporation yielded the desired product as a colourless, intensely lachrymatory liquid (2.0 g; 100%). The mixture was then cooled The product was extracted into ether (80 ml), which was washed with water and aqueous sodium bicarbonate solution dried over magnesium sulphate Evaporation

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

実験手順: 1,3-Difluorobenzene (2.02 g; 17.7 mM) and anhydrous aluminium chloride (2.60 g; 19.47 mM) were stirred together under dry nitrogen at room temperature. A solution of fluoroacetyl chloride (1,71 g; 17.7 mM) in anhydrous methylene chloride (2 ml) was added over 30 minutes. The mixture was then warmed at about 50° for 3 hours. On cooling methylene chloride (40 ml) was added and the mixture was poured onto ice. The methylene chloride layer was separated, dried over magnesium sulphate and evaporated to give a white solid. This material was chromatographed on a column of silica eluting with a mixture of hexane/methylene chloride (65:35 by volume). The product-containing fractions were collected. The title compound crystallised on evaporation of these fractions and was dried in a vacuum desiccator to a colourless crystalline solid (1.12 g; 36% yield), melting point 57°-8°. The mixture was then warmed at about 50° for 3 hours was added the mixture was poured onto ice The methylene chloride layer was separated dried over magnesium sulphate evaporated to give a white solid This material was chromatographed on a column of silica eluting with a mixture of hexane/methylene chloride (65:35 by volume) The product-containing fractions were collected The title compound crystallised on evaporation of these fractions was dried in a vacuum desiccator to a colourless crystalline solid (1.12 g; 36% yield), melting point 57°-8°