2-(3,4,5-trifluorophenyl)cyclohexan-1-one

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

実験手順: 2-(3,4,5-Trifluoro-phenyl)-cyclohexanone (100 mg, 0.44 mmol) was reacted with tert.-butoxy-bis-(dimethylamino)-methane using in analogous manner the procedure described in example 45a) to give crude title compound (123 mg) as a brown oil which was used directly in the next step. MS ISP (m/e): 284.2 (100) [(M+H)+].

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

実験手順: To a solution of 2-(3,4,5-trifluoro-phenyl)-cyclohexanol (215 mg, 0.93 mmol) dissolved in methylene chloride (15 mL) was added under nitrogen Dess-Martin reagent (475 mg, 1.1 mmol, 15 weight-percent in methylene chloride). The reaction was stirred at room temperature over night. The same amount of Des-Martin reagent was added and the reaction was stirred at room temperature over night. The reaction was poured onto a saturated sodium bicarbonate solution. The organic layer was washed with 10% aqueous sodium thiosulfate solution and brine, dried over sodium sulfate, filtered and the solvent was removed under reduced pressure. The residue was stirred with heptane/ethyl acetate (7:3 v/v) and the solid was filtered off to yield the title compound (202 mg, 95%) as a yellow solid. 1H NMR (CDCl3, 300 MHz): δ (ppm)=7.10-7.20 (m, 2H), 3.84 (dd, 1H), 2.28-2.33 (m, 2H), 1.65-2.12 (m, 6H). was added under nitrogen Dess-Martin reagent (475 mg, 1.1 mmol, 15 weight-percent in methylene chloride) The same amount of Des-Martin reagent was added the reaction was stirred at room temperature over night The organic layer was washed with 10% aqueous sodium thiosulfate solution and brine dried over sodium sulfate filtered the solvent was removed under reduced pressure The residue was stirred with heptane/ethyl acetate (7:3 v/v) the solid was filtered off