[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH2:9][C:10]2=[O:13])=[CH:5][CH:4]=1.[F:14][C:15]([F:22])([F:21])[C:16](OCC)=[O:17].[H-].[Na+].O1CCCC1>C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH:9]([C:16](=[O:17])[C:15]([F:22])([F:21])[F:14])[C:10]2=[O:13])=[CH:5][CH:4]=1A mixture of 7-methoxy-1-tetralone (7.8 g), ethyl trifluoroacetate (6 ml), sodium hydride (80% dispersion in mineral oil, 1.8 g) and tetrahydrofuran (75 ml) was stirred under reflux for 2 h under an atmosphere of argon. The cooled reaction mixture was treated with 20% acetic acid solution (250 ml) and the mixture was extracted twice with ethyl acetate. The extracts were combined, dried and evaporated to dryness under reduced pressure, and the residue was recrystallised from ethanol to give 7-methoxy-2-(2,2,2-trifluoracetyl)-1-tetralone, m.p. 89°-90°.
読み込み中…