反应详情

温度

60 °C

To a solution of ethyl 2-(tert-butoxy)-2-(3,5-dibromothiophen-2-yl)acetate (10c) (70 mg, 0.17 mmol) in tetrahydrofuran (1 mL) were added tripotassium phosphate (111 mg, 0.52 mmol), phenylboronic acid (23 mg, 0.19 mmol) and a solution of palladium acetate (1.2 mg, 5.2 μmol) and xantphos (3.0 mg, 5.2 μmol) in tetrahydrofuran (1 mL) previously stirred for 5 minutes. The reaction mixture was heated at 60° C. for 3 hours. The mixture was then filtered and the precipitate was rinsed with dichloromethane (5 mL). The filtrate was concentrated in vacuo. The residue was purified by flash chromatography (cyclohexane/ethyl acetate 80/20) to provide the desired product (10d) (45 mg, 0.11 mmol, 65%).

1. filtrationThe mixture was then filtered
2. washthe precipitate was rinsed with dichloromethane (5 mL)
3. concentrationThe filtrate was concentrated in vacuo
4. customThe residue was purified by flash chromatography (cyclohexane/ethyl acetate 80/20)