1,4-dibromo-1,1,2,2-tetrafluorobutane

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

実験手順: In 42 g of dimethyl sulfoxide were dissolved 10.0 g (0.035 mole) of 1,4-dibromo-1,1,2,2,-tetrafluorobutane and 5.0 g (0.035 mole) of sodium benzoate, which was stirred at 60° C. for 3.5 hours. The reaction solution was cooled to room temperature, after which toluene and water were added. The organic layer was taken out and washed once with 20 g of an aqueous saturated sodium hydrogen carbonate solution and twice with 20 g of an aqueous saturated sodium chloride solution. The organic layer was concentrated under reduced pressure, obtaining a compound, 4-bromo-3,3,4,4-tetrafluorobutyl benzoate. Colorless oily matter, 4.1 g. The reaction solution was cooled to room temperature washed once with 20 g of an aqueous saturated sodium hydrogen carbonate solution and twice with 20 g of an aqueous saturated sodium chloride solution The organic layer was concentrated under reduced pressure

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

実験手順: To a solution of 1.2 g of 1,4-dibromo-1,1,2,2-tetrafluorobutane and 1.0 g of methyl (3,3,3-trifluoropropylsulfonyl)acetate in 30 ml of dimethyl sulfoxide was added 0.2 g of sodium hydride (60% in oil) at room temperature. The mixture was stirred at the same temperature for 3 days. To the reaction mixture was added 10% hydrochloric acid, and then extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The obtained residue was subjected to silica gel chromatography to obtain 0.50 g of methyl 6-bromo-5,5,6,6-tetrafluoro-2-(3,3,3-trifluoropropylsulfonyl)hexanoate (hereinafter referred to as the present compound (4)). extracted with ethyl acetate The organic layer was washed with a saturated sodium chloride aqueous solution dried over anhydrous magnesium sulfate concentrated under reduced pressure

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In 42 g of dimethyl sulfoxide were dissolved 10.0 g (0.035 mole) of 1,4-dibromo-1,1,2,2-tetrafluorobutane and 5.0 g (0.035 mole) of sodium benzoate, which was stirred at 60° C. for 3.5 hours. The reaction solution was cooled to room temperature, after which toluene and water were added. The organic layer was taken out and washed once with 20 g of an aqueous saturated sodium hydrogen carbonate solution and twice with 20 g of an aqueous saturated sodium chloride solution. The organic layer was concentrated under reduced pressure, obtaining a compound, 4-bromo-3,3,4,4-tetrafluorobutyl benzoate. Colorless oily matter, 4.1 g. The reaction solution was cooled to room temperature washed once with 20 g of an aqueous saturated sodium hydrogen carbonate solution and twice with 20 g of an aqueous saturated sodium chloride solution The organic layer was concentrated under reduced pressure