反应详情

A mixture of 6-methoxytetralone (29.24 g, 165.9 mmol), paraformaldehyde (22.4 g, 746.6 mmol) and N-methylanilinium trifluoroactate (55 g, 248.9 mmol) in 250 mL THF was refluxed for 4 hours and allowed to come to room temperature. To this was added ether (250 mL) with stirring and the mixture was decanted to remove the gummy precipitate. The supernatant was washed with sat. NaHCO3, the oganic layer was dried (MgSO4) and concentrated. The residue was redissolved in ether, filtered through celite and concentrated to afford the title compound as a thick yellow oil.

1. temperaturewas refluxed for 4 hours
2. customto come to room temperature
3. customthe mixture was decanted
4. customto remove the gummy precipitate
5. washThe supernatant was washed with sat. NaHCO3
6. dry with materialthe oganic layer was dried (MgSO4)
7. concentrationconcentrated
8. dissolutionThe residue was redissolved in ether
9. filtrationfiltered through celite
10. concentrationconcentrated