反应详情

温度

80 °C

A mixture of methyl 7-bromo-2,3-dihydro-1-benzoxepine-4-carboxylate (1416 mg, 5.00 mmol), zinc cyanide (352 mg, 3.00 mmol), tetrakis(triphenylphosphine)palladium (347 mg, 0.30 mmol) and DMF(10 ml) was stirred at 80° C. for 3 hours. The mixture was concentrated under reduced pressure, and to the residue was added ethyl acetate. Insoluble materials were filtered off, which were washed with ethyl acetate. The filtrate was concentrated under reduced pressure. The resulting crude product was recrystallized from ethyl acetate to give methyl 7-cyano-2,3-dihydro-1-benzoxepine-4-carboxylate (800 mg, 3.49 mmol, 70%).

1. concentrationThe mixture was concentrated under reduced pressure
2. additionto the residue was added ethyl acetate
3. filtrationInsoluble materials were filtered off
4. washwhich were washed with ethyl acetate
5. concentrationThe filtrate was concentrated under reduced pressure
6. customThe resulting crude product was recrystallized from ethyl acetate