反应详情

To a solution of (6-bromo-naphthalen-2-yl)-(6,7-dimethoxy-quinolin-4-yl)-methanol (Step e, 0.55 g, 1.3 mmol) in formic acid (10 mL), was added Zn dust (500 mg, 7.6 mmol). The suspension was heated at reflux for 6 h and the solvent was removed in vacuo. The resulting residue was worked up with 1N NaOH and extracted with CH2Cl2 3×. The combined organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude was purified with silica gel column chromatography (40-65% EtOAc/Hexane) to give the titled compound. MS (ESI, pos. ion) m/z: 408.1 (M+1).

1. temperatureThe suspension was heated
2. temperatureat reflux for 6 h
3. customthe solvent was removed in vacuo
4. extractionextracted with CH2Cl2 3×
5. washThe combined organic layer was washed with water and brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe crude was purified with silica gel column chromatography (40-65% EtOAc/Hexane)