1-(2-fluoro-4-iodophenyl)ethanone

Conditions: temp:0.00; pressure:0.00; stir:

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

Procedure: A solution of bromine (2.74 mL, 53.18 mmol) in acetic acid (30 mL) was added dropwise to a solution of 1-(2-fluoro-4-iodo-phenyl)-ethanone (14.04 g, 53.18 mmol) in acetic acid (200 mL) at room temperature under an atmosphere of nitrogen and then stirred for 24 hours. The reaction was concentrated to near dryness in vacuo, diluted with ethyl acetate (200 mL) and basified with saturated aqueous sodium carbonate solution. The organic layer was washed with brine, dried over sodium sulfate, filtered through a pad of silica gel and concentrated in vacuo to give 2-bromo-1-(2-fluoro-4-iodo-phenyl)-ethanone (18.10 g, 99%). The reaction was concentrated diluted with ethyl acetate (200 mL) The organic layer was washed with brine dried over sodium sulfate filtered through a pad of silica gel concentrated in vacuo

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

Procedure: To a solution of 1-(2-fluoro-4-iodo-phenyl)-ethanol (15.50 g, 58.26 mmol) in dichloromethane (250 mL) was added manganese dioxide (101.26 g, 1.17 mole) and the reaction mixture was heated to reflux for 24 hours. The reaction mixture was cooled, filtered through a pad of celite coated with a thin layer of silica gel and concentrated in vacuo to give 1-(2-fluoro-4-iodo-phenyl)-ethanone (14.04 g, 91%). the reaction mixture was heated to reflux for 24 hours The reaction mixture was cooled filtered through a pad of celite coated with a thin layer of silica gel concentrated in vacuo

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

Procedure: A solution of bromine (2.74 mL, 53.18 mmol) in acetic acid (30 mL) was added dropwise to a solution of 1-(2-fluoro-4-iodo-phenyl)-ethanone (14.04 g, 53.18 mmol) in acetic acid (200 mL) at room temperature under an atmosphere of nitrogen and then stirred for 24 hours. The reaction was concentrated to near dryness in vacuo, diluted with ethyl acetate (200 mL) and basified with saturated aqueous sodium carbonate solution. The organic layer was washed with brine, dried over sodium sulfate, filtered through a pad of silica gel and concentrated in vacuo to give 2-bromo-1-(2-fluoro-4-iodo-phenyl)-ethanone (18.10 g, 99%). The reaction was concentrated diluted with ethyl acetate (200 mL) The organic layer was washed with brine dried over sodium sulfate filtered through a pad of silica gel concentrated in vacuo

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

Procedure: To a solution of 1-(2-fluoro-4-iodo-phenyl)-ethanol (15.50 g, 58.26 mmol) in dichloromethane (250 mL) was added manganese dioxide (101.26 g, 1.17 mole) and the reaction mixture was heated to reflux for 24 hours. The reaction mixture was cooled, filtered through a pad of celite coated with a thin layer of silica gel and concentrated in vacuo to give 1-(2-fluoro-4-iodo-phenyl)-ethanone (14.04 g, 91%). the reaction mixture was heated to reflux for 24 hours The reaction mixture was cooled filtered through a pad of celite coated with a thin layer of silica gel concentrated in vacuo