反应详情

To a refluxing solution of 2-tert-butyl-4-fluoro-6-nitrophenyl methyl carbonate (250 mg, 0.92 mmol) and ammonium formate (250 mg, 4 mmol) in EtOH (10 mL) was added 5% Pd—C (170 mg). The mixture was refluxed for additional 1 h, cooled and filtered through Celite. The solvent was removed by evaporation and the residue was purified by column chromatography (0-15%, EtOAc—Hexane) to give 2-tert-butyl-4-fluoro-6-aminophenyl methyl carbonate (C-6) (60 mg, 27%). HPLC ret. time 3.35 min, 10-99% CH3CN, 5 min run; ESI-MS 242.0 m/z (MH+).

1. temperatureThe mixture was refluxed for additional 1 h
2. temperaturecooled
3. filtrationfiltered through Celite
4. customThe solvent was removed by evaporation
5. customthe residue was purified by column chromatography (0-15%, EtOAc—Hexane)