反应详情

温度

200 °C

A mixture of 259 (420mg, 2.76 mmol), 2-fluoro-4-nitrophenol (651 mg, 4.14 mmol) and K2CO3(1.14 g, 8.28 mmol) in Ph2O (15 mL) was heated at 200° C. for 6 hours, cooled to room temperature and partitioned between EtOAc and water. Organic phase was collected, dried and concentrated. The residue was purified by flash column chromatography with gradient elution from hexane to hexane/EtOAc (3:1), to afford the title compound 260 (333 mg, 44% yield) as a yellowish solid. MS (m/z): 274.1(M+H) (found).

1. temperaturecooled to room temperature
2. custompartitioned between EtOAc and water
3. customOrganic phase was collected
4. customdried
5. concentrationconcentrated
6. customThe residue was purified by flash column chromatography with gradient elution from hexane to hexane/EtOAc (3:1)