4-fluoro-2-N-(2-fluorophenyl)benzene-1,2-diamine

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

実験手順: (5-Fluoro-2-nitrophenyl)-(2-fluorophenyl)amine (3.04 g, 12.16 mmol) was dissolved in EtOAc (120 mL) and the flask evacuated and flushed with nitrogen gas. 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas, at RT overnight. A further amount of 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h. The resultant mixture was filtered through Celite® and the filtrate concentrated in vacuo to afford the title compound as a dark yellow oil, which solidified on standing (2.89 g, 95%). 1H NMR (CDCl3, 400 MHz): δ 7.05-6.87 (2H, m), 6.83-6.68 (3H, m), 6.68-6.59 (2H, m), 5.36 (1H, s), 3.49 (2H, s) the flask evacuated flushed with nitrogen gas 10% Pd/C (0.3 g) was added A further amount of 10% Pd/C (0.3 g) was added the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h The resultant mixture was filtered through Celite® the filtrate concentrated in vacuo

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

実験手順: (5-Fluoro-2-nitrophenyl)-(2-fluorophenyl)amine (3.04 g, 12.16 mmol) was dissolved in EtOAc (120 mL) and the flask evacuated and flushed with nitrogen gas. 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas, at RT overnight. A further amount of 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h. The resultant mixture was filtered through Celite® and the filtrate concentrated in vacuo to afford the title compound as a dark yellow oil, which solidified on standing (2.89 g, 95%). 1H NMR (CDCl3, 400 MHz): δ 7.05-6.87 (2H, m), 6.83-6.68 (3H, m), 6.68-6.59 (2H, m), 5.36 (1H, s), 3.49 (2H, s) the flask evacuated flushed with nitrogen gas 10% Pd/C (0.3 g) was added A further amount of 10% Pd/C (0.3 g) was added the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h The resultant mixture was filtered through Celite® the filtrate concentrated in vacuo

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

実験手順: (5-Fluoro-2-nitrophenyl)-(2-fluorophenyl)amine (3.04 g, 12.16 mmol) was dissolved in EtOAc (120 mL) and the flask evacuated and flushed with nitrogen gas. 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas, at RT overnight. A further amount of 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h. The resultant mixture was filtered through Celite® and the filtrate concentrated in vacuo to afford the title compound as a dark yellow oil, which solidified on standing (2.89 g, 95%). 1H NMR (CDCl3, 400 MHz): δ 7.05-6.87 (2H, m), 6.83-6.68 (3H, m), 6.68-6.59 (2H, m), 5.36 (1H, s), 3.49 (2H, s) the flask evacuated flushed with nitrogen gas 10% Pd/C (0.3 g) was added A further amount of 10% Pd/C (0.3 g) was added the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h The resultant mixture was filtered through Celite® the filtrate concentrated in vacuo

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

実験手順: (5-Fluoro-2-nitrophenyl)-(2-fluorophenyl)amine (3.04 g, 12.16 mmol) was dissolved in EtOAc (120 mL) and the flask evacuated and flushed with nitrogen gas. 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas, at RT overnight. A further amount of 10% Pd/C (0.3 g) was added and the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h. The resultant mixture was filtered through Celite® and the filtrate concentrated in vacuo to afford the title compound as a dark yellow oil, which solidified on standing (2.89 g, 95%). 1H NMR (CDCl3, 400 MHz): δ 7.05-6.87 (2H, m), 6.83-6.68 (3H, m), 6.68-6.59 (2H, m), 5.36 (1H, s), 3.49 (2H, s) the flask evacuated flushed with nitrogen gas 10% Pd/C (0.3 g) was added A further amount of 10% Pd/C (0.3 g) was added the reaction mixture stirred under an atmosphere of hydrogen gas for an extra 2 h The resultant mixture was filtered through Celite® the filtrate concentrated in vacuo