反应详情

温度

90 °C

To a stirred solution of 5-Bromo-2-benzofuran-1(3H)-one (20 g, 94 mmol) in DMF (500 mL) was added Acrolein diethyl acetal (37 g, 282 mmol), Bu4NOAc (57 g, 188 mmol), K2CO3 (19.5 g, 141 mmol), KCl (7.0 g, 94 mmol) and Pd(OAc)2 (200 mg). The mixture was stirred for 2.5 hours at 90° C. After the mixture was cooled, 2 N HCl was slowly added and the resulting reaction mixture was stirred at room temperature for 10 min, and diluted with EtOAc, washed with water. The organic layer was dried over Na2SO4 and concentrated in vacuo. The residue was purified with silica gel chromatography (petrol ether/EtOAc=2:1) to give title product.

1. temperatureAfter the mixture was cooled
2. customthe resulting reaction mixture
3. stirringwas stirred at room temperature for 10 min
4. washwashed with water
5. dry with materialThe organic layer was dried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified with silica gel chromatography (petrol ether/EtOAc=2:1)