反应详情

温度

20 °C

To a solution of produce tert-butyl thiophen-2-ylmethylcarbamate (1.28 g, 6 mmol, 1.0 equiv.) in DMF (4 mL) was added NBS (1.17 g, 6.6 mmol, 1.1 eq). After stirring at 20° C. for 5 h, the reaction mixture was diluted with ethyl acetate and washed with water for three times. The organic layer was dried (MgSO4) and concentrated in vacua. The residue was purified by silica gel column chromatography (PE/EtOAc=100:1 to 5:1) to afford tert-butyl (5-bromothiophen-2-yl)methylcarbamate (1.6 g, 91%). LC-MS (m/z)=235.9 [M−55]+. 1H NMR (400 MHz, DMSO-d6): δ 1.39 (s, 9H), 4.20 (d, J=6.0 Hz, 2H), 6.76 (d, J=4.0 Hz, 1H), 7.03 (d, J=3.6 Hz, 1H), 7.52 (t, J=5.6 Hz, 1H).

1. washwashed with water for three times
2. dry with materialThe organic layer was dried (MgSO4)
3. concentrationconcentrated in vacua
4. customThe residue was purified by silica gel column chromatography (PE/EtOAc=100:1 to 5:1)