3-chloro-1-(4-fluorophenyl)propan-1-ol

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

実験手順: A catalytic amount (2 drops) of phosphorus oxytrichloride was added to 10 ml of an ethereal solution containing 277 mg of 3-chloro-1-(4-fluorophenyl)propanol and 330 mg of 2-(4-acetamidophenoxymethyl)-3,4-dihydro-2H-pyran and the mixture was allowed to react at room temperature for 8 days. The precipitated crystals were separated by filtration, giving 240 mg of the isomer of lesser polarity of the title compound, melting at 133°-135° C. to react at room temperature for 8 days The precipitated crystals were separated by filtration

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

実験手順: One drop of phosphorus oxytrichloride was added to a solution of 222 mg of 3-chloro-1-(4-fluorophenyl)propanol and 233 mg of 2-(4-fluorophenoxymethyl)-3,4-dihydro-2H-pyran in 5 ml of diethyl ether, and the mixture was stirred at room temperature for 2 days. At the end of this time, 2 drops of triethylamine were added, the solvent was evaporated off and the residue was purified by column chromatography through silica gel, to give 245 mg of the title compound. the solvent was evaporated off the residue was purified by column chromatography through silica gel

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

実験手順: A catalytic amount (2 drops) of phosphorus oxytrichloride was added to 10 ml of an ethereal solution containing 277 mg of 3-chloro-1-(4-fluorophenyl)propanol and 330 mg of 2-(4-acetamidophenoxymethyl)-3,4-dihydro-2H-pyran and the mixture was allowed to react at room temperature for 8 days. The precipitated crystals were separated by filtration, giving 240 mg of the isomer of lesser polarity of the title compound, melting at 133°-135° C. to react at room temperature for 8 days The precipitated crystals were separated by filtration

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

実験手順: One drop of phosphorus oxytrichloride was added to a solution of 222 mg of 3-chloro-1-(4-fluorophenyl)propanol and 233 mg of 2-(4-fluorophenoxymethyl)-3,4-dihydro-2H-pyran in 5 ml of diethyl ether, and the mixture was stirred at room temperature for 2 days. At the end of this time, 2 drops of triethylamine were added, the solvent was evaporated off and the residue was purified by column chromatography through silica gel, to give 245 mg of the title compound. the solvent was evaporated off the residue was purified by column chromatography through silica gel