反应详情

温度

80 °C

A mixture of 2-(7-bromoimidazo[1,2-b][1,2,4]triazin-3-yl)propan-2-ol (0.10 g, 0.38 mmol), 2,4-difluoro-3-(pyridin-4-yl)benzeneboronic acid (0.14 g, 0.58 mmol) and sodium carbonate (950 μL of a 2 M solution) in ethylene glycol dimethyl ether (2 ml) was degassed by bubbling nitrogen through for 20 min. Tetrakis(triphenylphosphine)palladium(0) (0.02 g, 0.02 mmol) was added and the mixture was degassed for a further 20 min before heating at 80° C. for 18 h. The mixture was filtered through glass fibre paper, and partitioned between ethyl acetate (30 ml) and water (30 ml). The organic layer was dried (Na2SO4), filtered and evaporated in vacuo. Purification by chromatography (silica gel, 5% MeOH/CH2C12), then recrystallisation from EtOAc/CH2C1 2, gave 7.0 mg (5%) of the title compound: 1H NMR (360 MHz, CDCl3) δ 7.19–7.24 (1H, s), 7.47 (2H, d, J 4.6), 8.14–8.21 (1H, m), 8.28 (1H, d, J 2.5), 8.77 (3H, dd, J 4.6, 6.0).

1. customwas degassed
2. customby bubbling nitrogen through for 20 min
3. customthe mixture was degassed for a further 20 min
4. filtrationThe mixture was filtered through glass fibre paper
5. custompartitioned between ethyl acetate (30 ml) and water (30 ml)
6. dry with materialThe organic layer was dried (Na2SO4)
7. filtrationfiltered
8. customevaporated in vacuo
9. customPurification by chromatography (silica gel, 5% MeOH/CH2C12)
10. customrecrystallisation from EtOAc/CH2C1 2