9-bromo-6,7,8,9-tetrahydrobenzo[7]annulen-5-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: 9-Bromo-6,7,8,9-tetrahydrobenzocyclohepten-5-one (590 mg, 2.5 mmol), 1-t-butoxycarbonylpiperazine (500 mg, 2.7 mmol) and potassium carbonate (510 mg, 3.7 mmol) were stirred overnight in DMF. The reaction solution was mixed with water, the reaction product was extracted with ethyl acetate, washed with water and saturated brine and dried with anhydrous sodium sulfate, the solvent was removed by evaporation under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 450 mg (1.3 mmol, 53%) of the title compound. the reaction product was extracted with ethyl acetate washed with water and saturated brine dried with anhydrous sodium sulfate the solvent was removed by evaporation under a reduced pressure the thus obtained material was separated purified by a silica gel column chromatography

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

実験手順: 9-Bromo-6,7,8,9-tetrahydrobenzocyclohepten-5-one (590 mg, 2.5 mmol), 1-t-butoxycarbonylpiperazine (500 mg, 2.7 mmol) and potassium carbonate (510 mg, 3.7 mmol) were stirred overnight in DMF. The reaction solution was mixed with water, the reaction product was extracted with ethyl acetate, washed with water and saturated brine and dried with anhydrous sodium sulfate, the solvent was removed by evaporation under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 450 mg (1.3 mmol, 53%) of the title compound. the reaction product was extracted with ethyl acetate washed with water and saturated brine dried with anhydrous sodium sulfate the solvent was removed by evaporation under a reduced pressure the thus obtained material was separated purified by a silica gel column chromatography

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

実験手順: 1-Benzosuberone (960 mg, 6.0 mmol), N-bromosuccinic acid imide (1.1 g, 6.3 mmol) and azobisisobutyronitrile (99 mg, 0.60 mmol) were stirred overnight at 80° C. in carbon tetrachloride (8 ml). The reaction solution was mixed with chloroform (60 ml), washed with saturated sodium bicarbonate aqueous solution and saturated brine and dried with anhydrous sodium sulfate, the solvent was removed by evaporation under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 770 mg (3.2 mmol, 54%) of the title compound. washed with saturated sodium bicarbonate aqueous solution and saturated brine dried with anhydrous sodium sulfate the solvent was removed by evaporation under a reduced pressure the thus obtained material was separated purified by a silica gel column chromatography