反应详情

温度

60 °C

A mixture of 2′,4′-difluoro-3-hydroxybiphenyl-4-carbaldehyde (8.00 g), iodoethane (8.98 g) and potassium carbonate (6.19 g) in acetone (70 mL) was stirred at 60° C. for 3 hours. The mixture was filtered through celite. The filtrate was concentrated in vacuo. The residue was diluted with ethyl acetate and water. The organic layer was separated and concentrated in vacuo. The residue was refluxed for 30 minutes in methanol (30 mL), cooled to room temperature, and further stirred for 1 hour. The solid was collected by filtration, washed with methanol (10 mL) and dried at 70° C. to give the title compound (5.16 g).

1. filtrationThe mixture was filtered through celite
2. concentrationThe filtrate was concentrated in vacuo
3. additionThe residue was diluted with ethyl acetate and water
4. customThe organic layer was separated
5. concentrationconcentrated in vacuo
6. temperatureThe residue was refluxed for 30 minutes in methanol (30 mL)
7. temperaturecooled to room temperature
8. stirringfurther stirred for 1 hour
9. filtrationThe solid was collected by filtration
10. washwashed with methanol (10 mL)
11. customdried at 70° C.