反应详情

温度

195 °C

Copper powder (100 g, 1.57 mol) is added to a solution of 6-bromo-benzo[b]-thiophene-2-carboxylic acid (1.04 Kg, 4.04 mol) in quinoline (2.5 L) at room temperature. The reaction mixture is heated to reflux (195° C.) for 10 h. The reaction mixture is cooled to room temperature and poured onto ice (2.5 Kg). Concentrated HCl (2.5 L) is added while stirring the resulting mass for 1 h. The reaction mixture is extracted with hexane (4×3 L) and washed with dilute HCl (1×2 L), aqueous bicarbonate (1×5 L), and brine solution (1×5 L). The layers are separated and the organic layer is dried over sodium sulfate and concentrated to give the title compound (0.54 Kg, 62%) as a light yellow solid.

1. temperatureThe reaction mixture is heated
2. temperatureThe reaction mixture is cooled to room temperature
3. additionpoured onto ice (2.5 Kg)
4. extractionThe reaction mixture is extracted with hexane (4×3 L)
5. washwashed with dilute HCl (1×2 L), aqueous bicarbonate (1×5 L), and brine solution (1×5 L)
6. customThe layers are separated
7. dry with materialthe organic layer is dried over sodium sulfate
8. concentrationconcentrated