反应详情

温度

160 °C

Combined ethyl 2-(4-bromophenyl)acetate (30 g, 0.123 mol) and NMP (200 mL). Then CuCN (33 g, 0.370 mol) was added in portions and then degassed and refilled with nitrogen three times. Then CuI (4.7 g, 0.0247 mol) was added in one portion. The reaction was degassed and refilled with nitrogen three times and then heated to 160° C. for 4 hours. Then the reaction was heated to 180° C. for another 3 hours. The solution was then cooled to room temperature and diluted with EtOAc (500 mL) and water (500 mL). After stirring for 10 mins, the reaction was filtered and the aqueous layer was extracted with EtOAc (500 mL×2). The combined organic layers were washed with brine, dried over Na2SO4 and concentrated to dryness to give the title compound (31 g, 66.5%) as a brown solid.

1. customdegassed
2. additionrefilled with nitrogen three times
3. customThe reaction was degassed
4. additionrefilled with nitrogen three times
5. temperatureThen the reaction was heated to 180° C. for another 3 hours
6. temperatureThe solution was then cooled to room temperature
7. additiondiluted with EtOAc (500 mL) and water (500 mL)
8. filtrationthe reaction was filtered
9. extractionthe aqueous layer was extracted with EtOAc (500 mL×2)
10. washThe combined organic layers were washed with brine
11. dry with materialdried over Na2SO4
12. concentrationconcentrated to dryness