反应详情

温度

90 °C

A mixture of 3-(3-bromo-2,6-difluorophenyl)pyridine (2.97 g, 11 mmol), potassium acetate (2.16 g, 22 mmol) and bis(neopentyl glycolato)diboron (2.86 g, 12.7 mmol) in 1,4-dioxane (30 ml) was heated at 90° C. for 16 h. The reaction was cooled, filtered (washing the filter cake with a small quantity of diethyl ether) and the filtrate concentrated in vacuo. The residue was partitioned between diethyl ether (100 ml) and 1 M sodium hydroxide (100 ml) and the organics discarded. The aqueous was washed with more diethyl ether and then cooled in an ice-water bath. The pH was adjusted to approximately 6 with 36% hydrochloric acid, and allowed to stand for 1 h. The resulting solid was collected by filtration and dried under vacuum to afford 2.2 g (85%) of the title compound as a grey solid: MS (ES+) m/z 236 [M+H]+.

1. temperatureThe reaction was cooled
2. filtrationfiltered (
3. washwashing the filter cake with a small quantity of diethyl ether) and the filtrate
4. concentrationconcentrated in vacuo
5. customThe residue was partitioned between diethyl ether (100 ml) and 1 M sodium hydroxide (100 ml)
6. washThe aqueous was washed with more diethyl ether
7. temperaturecooled in an ice-water bath
8. filtrationThe resulting solid was collected by filtration
9. customdried under vacuum