反应详情

To a solution of imidazole (15 mg) in 2 mL DME was added NaH (12 mg, 60% dispersion in mineral oil); a precipitate formed immediately. The mixture was stirred at room temp for 5 min, then heated to 75 C. A solution of 1-chloro-4-phenyl-6-methoxyisoquinoline-3-carbonitrile (60 mg) in 1 mL DME was added via cannula. Heating continued at 75 C for 45 min. The reaction was cooled to room temp and quenched by adding a few drops of water, then partitioned between saturated aqueous sodium bicarbonate and EtOAc. The organic solution was washed with brine (1×), dried over MgSO4 and concentrated. Flash chromatography (0% to 10% MeOH (10% NH4OH) in EtOAc) gave a white solid.

1. customa precipitate formed immediately
2. temperatureheated to 75 C
3. temperatureHeating
4. waitcontinued at 75 C for 45 min
5. temperatureThe reaction was cooled to room temp
6. customquenched
7. additionby adding a few drops of water
8. custompartitioned between saturated aqueous sodium bicarbonate and EtOAc
9. washThe organic solution was washed with brine (1×)
10. dry with materialdried over MgSO4
11. concentrationconcentrated
12. customFlash chromatography (0% to 10% MeOH (10% NH4OH) in EtOAc) gave a white solid