3-氟-3-甲基丁-2-one

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 3-methyl-3-fluoro-2-butanone (0.1031 g, 0.990 mmol) in anhydrous dichloromethane (5 ml) under nitrogen was added solid pyridinium tribromide (0.7035 g, 1.98 mmol) and the mixture was stirred at room temperature for 18 h. The mixture was then diluted with dichloromethane (5 ml), washed with dilute aqueous sodium hydrogensulfite (10 ml), then saturated aqueous NaCl (10 ml), dried (Na2SO4) and evaporated under low vacuum with no heat. The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)] to afford 0.1869 g (72%) of the title compound as a colourless oil: 1H NMR (360 MHz, CDCl3) δ 1.65 (6H, d, J 21.5 Hz), 6.51 (1H, d, J 1.5 Hz). washed with dilute aqueous sodium hydrogensulfite (10 ml) saturated aqueous NaCl (10 ml), dried (Na2SO4) evaporated under low vacuum with no heat The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)]

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 3-methyl-3-fluoro-2-butanone (0.1031 g, 0.990 mmol) in anhydrous dichloromethane (5 ml) under nitrogen was added solid pyridinium tribromide (0.7035 g, 1.98 mmol) and the mixture was stirred at room temperature for 18 h. The mixture was then diluted with dichloromethane (5 ml), washed with dilute aqueous sodium hydrogensulfite (10 ml), then saturated aqueous NaCl (10 ml), dried (Na2SO4) and evaporated under low vacuum with no heat. The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)] to afford 0.1869 g (72%) of the title compound as a colourless oil: 1H NMR (360 MHz, CDCl3) δ1.65 (6H, d, J 21.5 Hz), 6.51 (1H, d, J 1.5 Hz). washed with dilute aqueous sodium hydrogensulfite (10 ml) saturated aqueous NaCl (10 ml), dried (Na2SO4) evaporated under low vacuum with no heat The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)]

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 3-methyl-3-fluoro-2-butanone (0.1031 g, 0.990 mmol) in anhydrous dichloromethane (5 ml) under nitrogen was added solid pyridinium tribromide (0.7035 g, 1.98 mmol) and the mixture was stirred at room temperature for 18 h. The mixture was then diluted with dichloromethane (5 ml), washed with dilute aqueous sodium hydrogensulfite (10 ml), then saturated aqueous NaCl (10 ml), dried (Na2SO4) and evaporated under low vacuum with no heat. The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)] to afford 0.1869 g (72%) of the title compound as a colourless oil: 1H NMR (360 MHz, CDCl3) δ 1.65 (6H, d, J 21.5 Hz), 6.51 (1H, d, J 1.5 Hz). washed with dilute aqueous sodium hydrogensulfite (10 ml) saturated aqueous NaCl (10 ml), dried (Na2SO4) evaporated under low vacuum with no heat The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)]

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of 3-methyl-3-fluoro-2-butanone (0.1031 g, 0.990 mmol) in anhydrous dichloromethane (5 ml) under nitrogen was added solid pyridinium tribromide (0.7035 g, 1.98 mmol) and the mixture was stirred at room temperature for 18 h. The mixture was then diluted with dichloromethane (5 ml), washed with dilute aqueous sodium hydrogensulfite (10 ml), then saturated aqueous NaCl (10 ml), dried (Na2SO4) and evaporated under low vacuum with no heat. The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)] to afford 0.1869 g (72%) of the title compound as a colourless oil: 1H NMR (360 MHz, CDCl3) δ 1.65 (6H, d, J 21.5 Hz), 6.51 (1H, d, J 1.5 Hz). washed with dilute aqueous sodium hydrogensulfite (10 ml) saturated aqueous NaCl (10 ml), dried (Na2SO4) evaporated under low vacuum with no heat The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)]