3-氨基-5-氟-N-甲基苯甲酰胺

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

实验步骤: To a solution of 3-fluoro-N-methyl-5-nitrobenzamide (500 mg, 2.52 mmoL) in methanol (7.5 mL) was added Pd/C (30%) and the mixture was stirred at RT for 1 h. The reaction mixture was filtered through Celite® (diatomaceous earth), washed with methanol and concentrated under reduced. Purification by silica gel column chromatography provided 3-amino-5-fluoro-N-methylbenzamide (0.300 g, 75%) as a solid. The reaction mixture was filtered through Celite® (diatomaceous earth) washed with methanol concentrated under reduced Purification by silica gel column chromatography

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

实验步骤: To a roundbottom flask charged with 3-fluoro-N-methyl-5-nitrobenzamide (961 mg, 4.85 mmol) was added EtOH (16 mL). The resulting suspension was thoroughly purged with nitrogen prior to the addition of 10% Pd/C (43 mg, 0.485 mmol). The reaction mixture was purged with H2 (g), then stirred under 1 atm. H2 balloon at RT. After 2 d, the reaction mixture was filtered through Celite® (diatomaceous earth) with the aid of EtOH and the filtrate was dried under reduced pressure to afford 3-amino-5-fluoro-N-methylbenzamide (825 mg, 4.91 mmol, 100%). The resulting suspension was thoroughly purged with nitrogen The reaction mixture was purged with H2 (g) at RT the reaction mixture was filtered through Celite® (diatomaceous earth) with the aid of EtOH the filtrate was dried under reduced pressure

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

实验步骤: To a roundbottom flask charged with 3-fluoro-N-methyl-5-nitrobenzamide (961 mg, 4.85 mmol) was added EtOH (16 mL). The resulting suspension was thoroughly purged with nitrogen prior to the addition of 10% Pd/C (43 mg, 0.485 mmol). The reaction mixture was purged with H2 (g), then stirred under 1 atm. H2 balloon at RT. After 2 d, the reaction mixture was filtered through Celite® (diatomaceous earth) with the aid of EtOH and the filtrate was dried under reduced pressure to afford 3-amino-5-fluoro-N-methylbenzamide (825 mg, 4.91 mmol, 100%). The resulting suspension was thoroughly purged with nitrogen The reaction mixture was purged with H2 (g) at RT the reaction mixture was filtered through Celite® (diatomaceous earth) with the aid of EtOH the filtrate was dried under reduced pressure

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

实验步骤: To a solution of 3-fluoro-N-methyl-5-nitrobenzamide (500 mg, 2.52 mmoL) in methanol (7.5 mL) was added Pd/C (30%) and the mixture was stirred at RT for 1 h. The reaction mixture was filtered through Celite® (diatomaceous earth), washed with methanol and concentrated under reduced. Purification by silica gel column chromatography provided 3-amino-5-fluoro-N-methylbenzamide (0.300 g, 75%) as a solid. The reaction mixture was filtered through Celite® (diatomaceous earth) washed with methanol concentrated under reduced Purification by silica gel column chromatography

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

实验步骤: To a roundbottom flask charged with 3-fluoro-N-methyl-5-nitrobenzamide (961 mg, 4.85 mmol) was added EtOH (16 mL). The resulting suspension was thoroughly purged with nitrogen prior to the addition of 10% Pd/C (43 mg, 0.485 mmol). The reaction mixture was purged with H2 (g), then stirred under 1 atm. H2 balloon at RT. After 2 d, the reaction mixture was filtered through Celite® (diatomaceous earth) with the aid of EtOH and the filtrate was dried under reduced pressure to afford 3-amino-5-fluoro-N-methylbenzamide (825 mg, 4.91 mmol, 100%). The resulting suspension was thoroughly purged with nitrogen The reaction mixture was purged with H2 (g) at RT the reaction mixture was filtered through Celite® (diatomaceous earth) with the aid of EtOH the filtrate was dried under reduced pressure