反应详情

The carbonitrile 25B (2.3 g, 10.28 mmol) was dissolved in 80 ml of dimethoxyethane. To the solution were added 40 ml of water, sodium bicarbonate (3 equiv., 2.6 g), [4-(trifluoromethoxy)phenyl]boronic acid (1.2 equiv., 2.54 g) and the mixture was stirred at rt for 5′. The mixture was degassed and put under argon. A catalytic amount of tetrakispalladium was added and the mixture was heated at 100° C. overnight. The solvents were evaporated off and the residue was dissolved with ethyl acetate, washed with water and brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The crude was crystallized from ethyl acetate and petroleum ether to give a beige solid. (2.0 g, 55.5% yield)1HNMR (DMSO, 400 MHz) δ 3.61 (4H, m), 3.72 (4H, m), 7.20 (1H, s), 7.79 (1H, s), 7.82 (2H, d, J=8 Hz), 8.35 (2H, d, J=8 Hz)

1. customThe mixture was degassed
2. additionA catalytic amount of tetrakispalladium was added
3. temperaturethe mixture was heated at 100° C. overnight
4. customThe solvents were evaporated off
5. dissolutionthe residue was dissolved with ethyl acetate
6. washwashed with water and brine
7. dry with materialThe organic phase was dried over sodium sulfate
8. concentrationconcentrated under vacuum
9. customThe crude was crystallized from ethyl acetate and petroleum ether
10. customto give a beige solid