2-溴-3-氯苯胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To tert-butyl(2-bromo-3-chlorophenyl)carbamate (0.4 g) in DCM (20 mL) was added TFA (10 mL). The reaction mixture was stirred at RT for 3 hours and then concentrated. Water (10 mL) was added to the residue, and the mixture was extracted with DCM (2×20 mL). The organic phase was separated, washed with aqueous saturated NaHCO3 and saturated NaCl, dried over anhydrous Na2SO4, and concentrated to give the title compound as a solid (0.2 g, 77%). 1H NMR (400 MHz, CDCl3) δ 7.03-6.99 (1H, m), 6.85-6.83 (1H, d, J=8.0 Hz), 6.65-6.63 (1H, d, J=8.0 Hz), 4.25 (2H, s). concentrated Water (10 mL) was added to the residue the mixture was extracted with DCM (2×20 mL) The organic phase was separated washed with aqueous saturated NaHCO3 and saturated NaCl dried over anhydrous Na2SO4 concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To tert-butyl(2-bromo-3-chlorophenyl)carbamate (0.4 g) in DCM (20 mL) was added TFA (10 mL). The reaction mixture was stirred at RT for 3 hours and then concentrated. Water (10 mL) was added to the residue, and the mixture was extracted with DCM (2×20 mL). The organic phase was separated, washed with aqueous saturated NaHCO3 and saturated NaCl, dried over anhydrous Na2SO4, and concentrated to give the title compound as a solid (0.2 g, 77%). 1H NMR (400 MHz, CDCl3) δ 7.03-6.99 (1H, m), 6.85-6.83 (1H, d, J=8.0 Hz), 6.65-6.63 (1H, d, J=8.0 Hz), 4.25 (2H, s). concentrated Water (10 mL) was added to the residue the mixture was extracted with DCM (2×20 mL) The organic phase was separated washed with aqueous saturated NaHCO3 and saturated NaCl dried over anhydrous Na2SO4 concentrated