反应详情

温度

80 °C

A mixture of compound N-1 (1.6 g, 7.20 mmol), 3-aminophenylboronic acid hemisulfate (1.60 g, 8.60 mmol), Palladium tetrakis triphenylphosphine (0.25 g, 0.216 mmol), sodium carbonate (40 mL, 2M, 82 mmol) in DMF (100 mL) was stirred for 2 hrs at 80° C. overnight. The solvent was removed and the crude reaction product was taken up in ethyl acetate (40 mL). The solution was washed with 5% solution of hydrochloric acid (30 mL), then with saturated sodium chloride solution (30 mL), dried over sodium sulfate and evaporated. Purification of the residue on silica gel (1:1 hexanes-EtOAc) gave 0.790 g of compound N-2 (48% yield).

1. customThe solvent was removed
2. customthe crude reaction product
3. washThe solution was washed with 5% solution of hydrochloric acid (30 mL)
4. dry with materialwith saturated sodium chloride solution (30 mL), dried over sodium sulfate
5. customevaporated
6. customPurification of the residue on silica gel (1:1 hexanes-EtOAc)