反应详情

温度

95 °C

To a solution of compound 51a (5.8 g, 23 mmol) in AcOH (20 mL) was added Br2 (7.3 g, 46 mmol) dropwise at 95° C. The reaction mixture was stirred for another 30 min at 95° C. and allowed to cool to rt. Et2O (100 mL) was added. The solids formed were collected by filtration and washed with Et2O (2×30 mL) to obtain compound 51b as a yellow solid. Mass Spectrum (LCMS, ESI pos.): Calcd. for C9H8BrN3O: 254.0 (M+H). Found 254.1.

1. temperatureto cool to rt
2. customThe solids formed
3. filtrationwere collected by filtration
4. washwashed with Et2O (2×30 mL)