反应详情

温度

80 °C

After degassing with N2, a mixture of methyl 8-fluoro-7-methyl-4-(1-methyl-1H-pyrazol-4-yl)quinoline-2-carboxylate (7-17, 169.2 mg, 0.57 mmol), NBS (106 mg, 0.59 mmol) and benzoyl peroxide (13.7 mg, 0.057 mmol) in CCl4 (2.8 ml) was stirred at 80° C. After 5 h, the solvent was removed and the residue was partitioned between EtOAC and sat. NaHCO3. The organic layer was washed with water, dried over Na2SO4 and filtered. Concentration afforded the crude methyl 7-(bromomethyl)-8-fluoro-4-(1-methyl-1H-pyrazol-4-yl)quinoline-2-carboxylate, which was used without further purification (7-18). LRMS m/z (M+H)+ 378.2 found, 378.0 required.

1. customAfter degassing with N2
2. customthe solvent was removed
3. customthe residue was partitioned between EtOAC and sat. NaHCO3
4. washThe organic layer was washed with water
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationConcentration