反应详情

To a solution of 7-bromo-2-(1H-pyrazol-4-yl)quinoxaline (0.225 g, 0.808 mmol) in dry N,N-dimethylformamide (5 mL) under a nitrogen atmosphere was added 60 wt % sodium hydride (92 mg, 2.27 mmol) portionwise. After 5 minutes of stirring with purging, 2-dimethylaminoethylbromide (0.37 g, 0.908 mmol) was added and the reaction mixture stirred at rt for 30 min, concentrated in vacuo and taken into dichloromethane. The organic solution was washed with water (2×), dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by silica gel chromatography, eluting with 0-5% methanol in ethyl acetate to furnish the title compound (0.183 g, 66% yield). ESMS m/e: 345.9; 347.8 [M]+.

1. customwith purging
2. stirringthe reaction mixture stirred at rt for 30 min
3. concentrationconcentrated in vacuo
4. washThe organic solution was washed with water (2×)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was purified by silica gel chromatography
9. washeluting with 0-5% methanol in ethyl acetate