反应详情

温度

80 °C

A mixture of Compound 261a (111 mg, 0.345 mmol), cupric sulphate (11 mg, 0.69 mmol), 1,10-phenantroline (24.9 mg, 0.138 mmol), K2CO3 (95.4 mg, 0.69 mmol), 2-pyrrolidone (39.7 μl, 0.518 mmol) and 5 mL of toluene was stirred at 80° C. for 12 h. The reaction mixture was cooled to r.t., diluted with EtOAc, washed with water, dried over Na2SO4 and evaporated to dryness in vacuo. The crude residue was purified by automated flash liquid chromatography (Horizon™-Biotage) eluting with PE-EtOAc gradient from 98:2 to 0:10, giving the title product (2 mg)

1. temperatureThe reaction mixture was cooled to r.t.
2. washwashed with water
3. dry with materialdried over Na2SO4
4. customevaporated to dryness in vacuo
5. customThe crude residue was purified by automated flash liquid chromatography (Horizon™-Biotage)
6. washeluting with PE-EtOAc gradient from 98:2 to 0:10