反应详情

温度

30 °C

Solid 3-aminobenzeneboronic acid (0.143 g, 0.92 mmol) was added to a solution of the mono triflate (17)(0.619 g, 0.58 mmol), sodium carbonate (195 mg, 1.84 mmol) and palladium tetrakis triphenylphosphine (26.6 mg, 0.023 mmol) in toluene (10 mL), ethanol (5 mL) and water (5 mL). The reaction mixture was allowed to stir at room temperature for overnight at 30° C. The reaction mixture was then partitioned between ethyl acetate and water. The organic layer was washed with water and brine and dried over magnesium sulphate. Excess solvent was removed by rotary evaporation under reduced pressure and the resulting residue was subjected to flash column chromatography (silica gel; gradient elution EtOAc/hexane 70/3085/15). Removal of excess eluent from selected fractions afforded the desired product (0.502 g, 0.49 mmol, 85%).

1. customThe reaction mixture was then partitioned between ethyl acetate and water
2. washThe organic layer was washed with water and brine
3. dry with materialdried over magnesium sulphate
4. customExcess solvent was removed by rotary evaporation under reduced pressure
5. washthe resulting residue was subjected to flash column chromatography (silica gel; gradient elution EtOAc/hexane 70/3085/15)
6. customRemoval of excess eluent