反应详情

温度

80 °C

To a solution of compound 18a (15.0 g, 51.2 mmol) in MeOH (100 mL) was added Fe (9.06 g, 162 mmol) and saturated NH4Cl solution (100 mL). The resulting solution was stirred at 80° C. for 5 h. After cooling to rt, the mixture was extracted with EtOAc (200 mL). The organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with EtOAc/petroleum ether (1:5 v/v) to obtain compound 18b as a black solid (13.0 g, 97% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C14H20N2O2: 249.2 (M+H). Found 249.0.

1. temperatureAfter cooling to rt
2. extractionthe mixture was extracted with EtOAc (200 mL)
3. washThe organic layer was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by flash column chromatography on silica gel
7. washeluting with EtOAc/petroleum ether (1:5 v/v)