3,5-difluorobenzoyl chloride

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: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: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:; See reaction.notes.procedure_details.

実験手順: To a solution of 2-amino-1-[3-(4-phenyl-piperidin-1-yl)-pyrrolidin-1-yl]-ethanone (preparation #9) (0.026 g, 0.09 mmol) and triethylamine (0.025 mL, 0.18 mmol) in DCM (0.7 mL) was added a solution of 3,5-difluoro-benzoyl chloride (0.016 g, 0.09 mmol) in dichloromethane (0.2 mL). The reaction mixture was stirred at ambient temperature for about 3 h then concentrated in vacuo. The residue was purified by flash chromatography on silica gel using 10% MeOH/EtOAc as the mobile phase to give 3,5-difluoro-N-{2-oxo-2-[3-(4-phenyl-piperidin-1-yl)-pyrrolidin-1-yl]-ethyl}-benzamide (0.021 g, 55%). RP-HPLC (Table 1, Method b) Rt 1.51 min; m/z: (M+H)+ 428. then concentrated in vacuo The residue was purified by flash chromatography on silica gel using 10% MeOH/EtOAc as the mobile phase