2-Azido-1-(4-bromophenyl)ethanone

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

実験手順: To a solution of compound 2-azido 4′-bromoacetophenone (1.0 g, 4.17 mmol) in MeOH (20 mL), Pd/C (10%, 100 mg) was added to the solution. The mixture was degassed and stirred under hydrogen system for 4 hours. The mixture was filtered and evaporated in vacuo without further purification to obtain 2-amino 4′-bromoacetophenone (0.535 g, 2.499 mmol, 60% yield). 1H NMR (d-MeOH) 4.63 (d, J=4.8 Hz, 2H), 7.62 (d, J=7.2 Hz, 2H), 8.03 (d, J=7.2 Hz, 2H) ppm. The mixture was degassed The mixture was filtered evaporated in vacuo without further purification

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

実験手順: A solution of 2,4′-dibromoacetophenone (1.390 g, 5.0 mmol) in MeOH (10 mL) was poured over 10 mL of an aqueous solution of sodium azide (0.325 g, 5.00 mmol) in an ice bath. The mixture was stirred at room temperature for 18 hours. The solvent was removed and then extracted with ethyl ether (20 mL) and water (20 mL). The organic layer was dried over MgSO4 and concentrated in vacuo to obtain 2-azido 4′-bromoacetophenone (1.0 g, 4.17 mmol, 83% yield). 1H NMR (CDCl3) 5.45 (s, 2H), 7.67 (d, J=8.4 Hz, 2H), 7.79 (d, J=8.4 Hz, 2H) ppm. The solvent was removed extracted with ethyl ether (20 mL) and water (20 mL) The organic layer was dried over MgSO4 concentrated in vacuo