反应详情

温度

90 °C

A mixture of 2-bromopyrimidine (2.0 g, 12.7 mmol), 4-bromo-2,3-difluorobenzeneboronic acid (1.0 g, 4.22 mmol), potassium carbonate (2.93 g, 21.1 mmol) in a mixture of toluene (30 ml)/ethanol (30 ml)/water (15 ml) were purged with nitrogen for 15 min. Tetrakis(triphenylphosphine)palladium(0) (488 mg, 0.42 mmol) was added and the mixture was stirred at 90° C. in a sealed-tube for overnight. The mixture was cooled to r.t. and was diluted with water and ethyl acetate. Layers were separated. The separated organic layer was dried (MgSO4), filtered and solvents were removed in vacuum. Column purification [Hexanes-Ethyl acetate, 2:1 (v/v)] gave bromide 3AC (0.97 g, 85%) as white solid.

1. customwere purged with nitrogen for 15 min
2. temperatureThe mixture was cooled to r.t.
3. customLayers were separated
4. dry with materialThe separated organic layer was dried (MgSO4)
5. filtrationfiltered
6. customsolvents were removed in vacuum
7. customColumn purification [Hexanes-Ethyl acetate, 2:1 (v/v)]