反应详情

温度

40 °C

NBS (9.53 g, 53.6 mmol) was added portionwise to a solution of 3-thiopheneethanol 6.87 g, 53.6 mmol) in AcOH (30 ml). The temperature was raised to 40° C. and mixture was stirred for 1 h. DCM (400 ml) and water was added. The organic layer was washed with water and sat. NaHCO3. The organic layer evaporated and residue purified by flash chromatography using 25-33% EtOAc in iso-hexane. Yield: 5.39 g (49%); colourless oil. 1H NMR (400 MHz, CDCl3): δ 2.89 (t, J 6.4 Hz, 2H), 3.85 (t, J 6.4 Hz, 2H), 6.89 (d, J 5.6 Hz, 1H), 7.26 (d, J 5.6 Hz, 1H).

1. washThe organic layer was washed with water and sat. NaHCO3
2. customThe organic layer evaporated
3. customresidue purified by flash chromatography