反应详情

8-Fluoro-2-formyl-5-methoxy-1-tetralone (20 g) was dissolved in dioxan. 2,3-Dichloro-5,6-dicyanobenzoquinone (21 g) was added and the mixture was heated under reflux for 2 hours. The mixture was allowed to cool and was filtered to remove solids. The solvent was removed under reduced pressure and the residue taken up in ethyl acetate. The product solution was washed with saturated NaHCO3 (aq) (×3), dried (MgSO4), filtered and evaporated to give a dark solid. This material was recrystallised from ethyl acetate/hexane to give 1-hydroxy-5-methoxy-8-fluoro-2-naphthaldehyde, m.p. 156°-158° C.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 2 hours
3. temperatureto cool
4. filtrationwas filtered
5. customto remove solids
6. customThe solvent was removed under reduced pressure
7. washThe product solution was washed with saturated NaHCO3 (aq) (×3)
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customevaporated
11. customto give a dark solid
12. customThis material was recrystallised from ethyl acetate/hexane