反应详情

4,5-Dihydro-thieno[2,3-c]pyrrol-6-one (0.365 g, 2.63 mmol) is dissolved in acetonitrile (10 mL), and NBS (0.47 g, 2.63 mmol) is slowly added at −10° C. The reaction mixture is stirred at room temperature overnight. The solvent is removed in vacuo and the residue taken-up in EtOAc and washed with 1M NaOH. The organic phase is dried over MgSO4, filtered and concentrated in vacuo. The crude is purified by silica gel column chromatography eluting with a 50:50 mixture and then 50:70 petroleum ether-EtOAc. The title compound is isolated (91.1 mg, 16%). HPLC (254 nm): Rt 2.55 min (70.3%), m/z 218/220 (M+H)+.

1. customThe solvent is removed in vacuo
2. washthe residue taken-up in EtOAc and washed with 1M NaOH
3. dry with materialThe organic phase is dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude is purified by silica gel column chromatography
7. washeluting with a 50:50 mixture