反应详情

To a solution of compound 1e (10.0 g, 32.1 mmol, as prepared in Example 1, Step E) in DMSO (50 mL) was added IBX (5.54 g, 19.7 mmol) in portions. The reaction mixture was stirred at rt for 3 h, and was quenched with 2N NaOH solution (50 mL). The resulting mixture was extracted with DCM (3×25 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel with EtOAc/petroleum ether (1:2 v/v) to obtain compound 2a as a yellow solid (6.00 g, 54% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C11H11BrN4O2: 311.0 (M+H). found 311.2.

1. customwas quenched with 2N NaOH solution (50 mL)
2. extractionThe resulting mixture was extracted with DCM (3×25 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by flash column chromatography on silica gel with EtOAc/petroleum ether (1:2 v/v)