反应详情

温度

-20 °C

To a solution of compound 1d (2.40 g, 10.3 mmol) in ACN (200 mL) was added NBS (2.40 g, 13.5 mmol) in portions at −20° C. The resulting solution was stirred at −20° C. for 2 h, and was concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with EtOAc/petroleum ether (1:1 v/v) to obtain compound 1e as a yellow solid (1.48 g, 41% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C11H13BrN4O2: 313.0 (M+H). Found 313.2.

1. concentrationwas concentrated under reduced pressure
2. customThe residue was purified by flash column chromatography on silica gel
3. washeluting with EtOAc/petroleum ether (1:1 v/v)