反应详情

温度

80 °C

A mixture of 2.53 g (10.1 mmol) of 2-fluoro-6-iodo benzaldehyde, 1.0 g (11.1 mmol) of mercapto-2-propanone and 3.5 mL (2.5 g, 25 mmol) of Et3N in 15 mL of DMSO was heated to 80° C. overnight. After cooling to room temperature, water was added and the mixture was extracted with ethyl acetate. The organic layer was washed with water (2 times), brine and dried over MgSO4. After evaporation of the solvents, the crude product was purified over silica gel column chromatography to afford 1.85 g (6.12 mmol, yield: 61%) of 2-acetyl-4-iodo benzo[b]thiophene as an orange powder. 1H-NMR (CDCl3), δ: 7.97 (s, 1H), 7.83 (d, J=7.9 Hz, 2H), 7.16 (t, J=7.9 Hz, 1H), 2.70 (s, 3H).

1. temperatureAfter cooling to room temperature
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with water (2 times), brine
4. dry with materialdried over MgSO4
5. customAfter evaporation of the solvents
6. customthe crude product was purified over silica gel column chromatography