反应详情

温度

80 °C

To a solution of (ii) (1.08 g, 3.67 mmol) in DMF (15 mL) was added N-bromosuccinimide (780 mg, 4.40 mmol) and the resulting mixture stirred at 80° C. for 1.5 h. The reaction mixture was then cooled to RT and the solvent was removed under reduced pressure. The residue was dissolved in EtOAc (100 mL) and washed with aq. saturated sodium bicarbonate (20 mL) and brine (20 mL). The organic phase was dried (MgSO4) and the volatiles removed in vacuo to give (iii) (1.37 g, >99%). ESI-MS: calculated [M+H]+ 373.0/375.0, observed [M+H]+ 373.1/375.1.

1. temperatureThe reaction mixture was then cooled to RT
2. customthe solvent was removed under reduced pressure
3. dissolutionThe residue was dissolved in EtOAc (100 mL)
4. washwashed with aq. saturated sodium bicarbonate (20 mL) and brine (20 mL)
5. dry with materialThe organic phase was dried (MgSO4)
6. customthe volatiles removed in vacuo