反应详情

温度

100 °C

To a solution of 1-fluoro-4-nitrobenzene (3.0 g, 21 mmol) and tert-butyl (2S)-2-amino-3-methylbutanoate hydrochloride (5.4 g, 26 mmol) in DMSO (20 mL) was added K2CO3 (8.8 g, 64 mmol). The reaction mixture was stirred at 100° C. for 8 h. EtOAc (200 mL) was added. The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (EtOAc/petroleum ether (1:10 v/v)) to obtain compound 55a as a yellow solid. Mass Spectrum (LCMS, ESI pos.): Calcd. for C15H22N2O4: 295.2 (M+H). Found 295.2.

1. washThe organic layer was washed with water and brine
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by flash column chromatography on silica gel (EtOAc/petroleum ether (1:10 v/v))