反应详情

180 g of 1-bromo-4-[2-(2-methoxyvinyl)phenyl]naphthalene and 1.0 L of dichloromethane were placed. 25 mL of methanesulfonic acid was added at room temperature while stirring. The stirring was conducted for 8 hours at room temperature. After the completion of the reaction, 1 L of an aqueous solution of 10% potassium carbonate was added. After removing an aqueous phase, an organic phase was washed with water and saturated saline, and dried with magnesium sulfate. After filtering off magnesium sulfate, the organic phase was concentrated. The residues were purified by silica gel column chromatography, whereby 24.4 g (yield 15%) of 5-bromobenzo[c]phenanthrene as an intended product was obtained.

1. additionwas added
2. customAfter removing an aqueous phase
3. washan organic phase was washed with water and saturated saline
4. dry with materialdried with magnesium sulfate
5. filtrationAfter filtering off magnesium sulfate
6. concentrationthe organic phase was concentrated