1-(2,4-difluorophenyl)-2-methylpropan-1-one

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: In 260 ml of methylene chloride was dissolved 145.5 g (0.79 mol) of 1-(2,4-difluorophenyl)-2-methylpropan-1-one, and 134.2 g (0.84 mol) of bromine was slowly added dropwise thereto at 20° C. or lower. The mixture was warmed to room temperature and stirred for 1 hour. A saturated sodium chloride aqueous solution and a saturated sodium thiosulfate aqueous solution were added to the reaction mixture. The organic layer was separated, washed successively with a saturated sodium chloride aqueous solution, a saturated sodium hydrogencarbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure to obtain 205.7 g (99%) of 2-bromo-1-(2,4-difluorophenyl)-2-methylpropan-1-one as a pale yellow oily substance. was slowly added dropwise at 20° C. The organic layer was separated washed successively with a saturated sodium chloride aqueous solution a saturated sodium hydrogencarbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried The solvent was removed by distillation 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 mixture of 120 g (0.68 mmol) of 2,4-difluorobenzoyl chloride, 3.7 g (37 mmol) of copper (I) chloride, and 400 ml of diethyl ether was added dropwise 442 ml of diethyl ether containing 130.2 g (0.88 mol) of isopropylmagnesium bromide at -25° C. over 4 hours. The temperature was elevated up to -5° C., and the mixture was stirred at that temperature for 30 minutes. To the reaction mixture were added dropwise 150 ml of water and then 120 ml of 6N hydrochloric acid. The organic layer was separated, washed successively with 5% hydrochloric acid, a saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure, and the residue was distilled under reduced pressure to obtain 104.3 g (83%) of 1-(2,4-difluorophenyl)-2-methylpropan-1-one as a colorless oily substance. was elevated up to -5° C. The organic layer was separated washed successively with 5% hydrochloric acid a saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried The solvent was removed by distillation under reduced pressure the residue was distilled 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 mixture of 120 g (0.68 mmol) of 2,4-difluorobenzoyl chloride, 3.7 g (37 mmol) of copper (I) chloride, and 400 ml of diethyl ether was added dropwise 442 ml of diethyl ether containing 130.2 g (0.88 mol) of isopropylmagnesium bromide at -25° C. over 4 hours. The temperature was elevated up to -5° C., and the mixture was stirred at that temperature for 30 minutes. To the reaction mixture were added dropwise 150 ml of water and then 120 ml of 6N hydrochloric acid. The organic layer was separated, washed successively with 5% hydrochloric acid, a saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure, and the residue was distilled under reduced pressure to obtain 104.3 g (83%) of 1-(2,4-difluorophenyl)-2-methylpropan-1-one as a colorless oily substance. was elevated up to -5° C. The organic layer was separated washed successively with 5% hydrochloric acid a saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried The solvent was removed by distillation under reduced pressure the residue was distilled under reduced pressure

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

実験手順: In 260 ml of methylene chloride was dissolved 145.5 g (0.79 mol) of 1-(2,4-difluorophenyl)-2-methylpropan-1-one, and 134.2 g (0.84 mol) of bromine was slowly added dropwise thereto at 20° C. or lower. The mixture was warmed to room temperature and stirred for 1 hour. A saturated sodium chloride aqueous solution and a saturated sodium thiosulfate aqueous solution were added to the reaction mixture. The organic layer was separated, washed successively with a saturated sodium chloride aqueous solution, a saturated sodium hydrogencarbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure to obtain 205.7 g (99%) of 2-bromo-1-(2,4-difluorophenyl)-2-methylpropan-1-one as a pale yellow oily substance. was slowly added dropwise at 20° C. The organic layer was separated washed successively with a saturated sodium chloride aqueous solution a saturated sodium hydrogencarbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried The solvent was removed by distillation 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 mixture of 120 g (0.68 mmol) of 2,4-difluorobenzoyl chloride, 3.7 g (37 mmol) of copper (I) chloride, and 400 ml of diethyl ether was added dropwise 442 ml of diethyl ether containing 130.2 g (0.88 mol) of isopropylmagnesium bromide at -25° C. over 4 hours. The temperature was elevated up to -5° C., and the mixture was stirred at that temperature for 30 minutes. To the reaction mixture were added dropwise 150 ml of water and then 120 ml of 6N hydrochloric acid. The organic layer was separated, washed successively with 5% hydrochloric acid, a saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation under reduced pressure, and the residue was distilled under reduced pressure to obtain 104.3 g (83%) of 1-(2,4-difluorophenyl)-2-methylpropan-1-one as a colorless oily substance. was elevated up to -5° C. The organic layer was separated washed successively with 5% hydrochloric acid a saturated sodium chloride aqueous solution, a saturated sodium carbonate aqueous solution, and a saturated sodium chloride aqueous solution, and dried The solvent was removed by distillation under reduced pressure the residue was distilled under reduced pressure