反应详情

Combine 8-methyl-quinoline (1.0 g, 6.99 mmol), NBS (1.3 g, 7.13 mmol), benzoyl peroxide (6.0 mg, 0.03 mmol), carbon tetrachloride (30 mL) and reflux for 17 h. Cool the reaction mixture to ambient temperature and evaporate the solvent. Dissolve the residue in chloroform (30 mL), wash the organic solution with saturated aqueous NaHCO3 (2×10 mL), brine (10 mL) and dry over anhydrous Na2SO4. Evaporate the solvent and purify by chromatography on silica gel eluting with DCM to obtain the title compound as a white solid (1.3 g, 83%). MS (ES+) m/z: 223 (M+H)+.

1. customevaporate the solvent
2. dissolutionDissolve the residue in chloroform (30 mL)
3. washwash the organic solution with saturated aqueous NaHCO3 (2×10 mL), brine (10 mL)
4. dry with materialdry over anhydrous Na2SO4
5. customEvaporate the solvent
6. custompurify by chromatography on silica gel eluting with DCM