1,1,1-trifluoro-5-phenylpentan-2-one

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:; See reaction.notes.procedure_details.

実験手順: 19.5 g (90 mmol) of said product (14-1) was dissolved in 200 ml of ethanol, and the solution was added with 1.7 g (45 mmol) of sodium borohydride and stirred at room temperature for 2 hours. The reaction mixture was poured into water and extracted with ethyl acetate, and the resultantly formed organic layer was washed with water and brine successively, then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 19.1 g of 5-phenyl-1,1,1-trifluoro-2-pentanol (15-1) as a colorless liquid. Yield: 97%. extracted with ethyl acetate the resultantly formed organic layer was washed with water and brine successively dried over anhydrous magnesium sulfate concentrated under reduced pressure

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

実験手順: 19.5 g (90 mmol) of said product (14-1) was dissolved in 200 ml of ethanol, and the solution was added with 1.7 g (45 mmol) of sodium borohydride and stirred at room temperature for 2 hours. The reaction mixture was poured into water and extracted with ethyl acetate, and the resultantly formed organic layer was washed with water and brine successively, then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 19.1 g of 5-phenyl-1,1,1-trifluoro-2-pentanol (15-1) as a colorless liquid. Yield: 97%. extracted with ethyl acetate the resultantly formed organic layer was washed with water and brine successively dried over anhydrous magnesium sulfate concentrated under reduced pressure

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

実験手順: Into a four-necked flask equipped with a thermometer, a dropping funnel and a stirrer, 4.8 g (0.2 mol) of magnesium flasks and 100 ml of anhydrous tetrahydrofuran were placed, followed by addition of a mixture of 4.0 g (20 mmol) of 1-bromo-3-phenylpropane and 10 ml of anhydrous tetrahydrofuran and a small quantity of iodine, heating of the flask contents to 60° C. and dropwise addition of a mixture of 35.8 g (0.18 mol) of 1-bromo-3-phenylpropane and 90 ml of anhydrous tetrahydrofuran at the same temperature. Thereafter, the mixture was stirred under reflux for 2 hours and then cooled to room temperature. The resulting mixture was added dropwise into a mixture consisting of 31.3 g (0.22 mol) of ethyl trifluoroacetate and 200 ml of anhydrous tetrahydrofuran. Thereafter, the mixture was stirred at -78° C. for 2 hours, then heated gradually to -50° C. and further stirred at the same temperature for 2 hours. Thereafter, 100 ml of 1N hydrochloric acid was added at -50° C., followed by heating to room temperature. The reaction mixture was extracted with 300 ml of ether and the formed organic layer was washed with water, a 5% sodium bicarbonate solution and brine successively in that order, then dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (eluent: toluene/hexane (1/4)) to give 20.3 g of 5-phenyl-1,1,1-trifluoropentane-2-one (14-1) in a yield of 47%. under reflux for 2 hours The resulting mixture was added dropwise into a mixture Thereafter, the mixture was stirred at -78° C. for 2 hours heated gradually to -50° C. further stirred at the same temperature for 2 hours by heating to room temperature The reaction mixture was extracted with 300 ml of ether the formed organic layer was washed with water a 5% sodium bicarbonate solution and brine successively in that order, then dried over anhydrous magnesium sulfate concentrated under reduced pressure

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

実験手順: Into a four-necked flask equipped with a thermometer, a dropping funnel and a stirrer, 4.8 g (0.2 mol) of magnesium flasks and 100 ml of anhydrous tetrahydrofuran were placed, followed by addition of a mixture of 4.0 g (20 mmol) of 1-bromo-3-phenylpropane and 10 ml of anhydrous tetrahydrofuran and a small quantity of iodine, heating of the flask contents to 60° C. and dropwise addition of a mixture of 35.8 g (0.18 mol) of 1-bromo-3-phenylpropane and 90 ml of anhydrous tetrahydrofuran at the same temperature. Thereafter, the mixture was stirred under reflux for 2 hours and then cooled to room temperature. The resulting mixture was added dropwise into a mixture consisting of 31.3 g (0.22 mol) of ethyl trifluoroacetate and 200 ml of anhydrous tetrahydrofuran. Thereafter, the mixture was stirred at -78° C. for 2 hours, then heated gradually to -50° C. and further stirred at the same temperature for 2 hours. Thereafter, 100 ml of 1N hydrochloric acid was added at -50° C., followed by heating to room temperature. The reaction mixture was extracted with 300 ml of ether and the formed organic layer was washed with water, a 5% sodium bicarbonate solution and brine successively in that order, then dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (eluent: toluene/hexane (1/4)) to give 20.3 g of 5-phenyl-1,1,1-trifluoropentane-2-one (14-1) in a yield of 47%. under reflux for 2 hours The resulting mixture was added dropwise into a mixture Thereafter, the mixture was stirred at -78° C. for 2 hours heated gradually to -50° C. further stirred at the same temperature for 2 hours by heating to room temperature The reaction mixture was extracted with 300 ml of ether the formed organic layer was washed with water a 5% sodium bicarbonate solution and brine successively in that order, then dried over anhydrous magnesium sulfate concentrated under reduced pressure