反应详情

温度

80 °C

To the solution of 8-7 (20 g, 44.0 mmol) in anhydrous DMF (250 mL) was added Pd(OAc)2 (2.0 g, 8.8 mmol), Bu4NBr (14.3 g, 44.0 mmol) and DIPEA (14.2 g, 110 mmol) under N2. The mixture was stirred at 80° C. for 3 h. TLC showed that the reaction was completed. The mixture was poured into ice water and extracted with ethyl acetate (150 mL×3). The organic layers were combined and were concentrated in vacuo. The residue was purified by flash chromatography (Silica-gel, petroleum ether/ethyl acetate=10:1) to afford 8-8 (13.0 g, 79%) as a white solid.

1. extractionextracted with ethyl acetate (150 mL×3)
2. concentrationwere concentrated in vacuo
3. customThe residue was purified by flash chromatography (Silica-gel, petroleum ether/ethyl acetate=10:1)