反应详情

Compound 4-(4-Fluoro-phenyl)-4-hydroxy-cyclohexanone ethylene ketal (8.23 g, 32.6 mmol) from Step 1 was stirred in TFA (25 mL) for 15 minutes. The reaction mixture was poured into H2O (100 mL) and then extracted with CHCl3 (2×75 mL). The organic solution was washed with saturated bicarbonate, dried (Na2SO4), filtered and concentrated under reduced pressure to afford crude 1-(4-fluorophenyl)-cyclohexen-4-one (6.44 g): 1H NMR (300 MHz, CDCl3) δ 7.35 (dd, J=8, 8 Hz, 2H), 7.04 (dd, J=8, 8 Hz, 2H), 6.05 (m, 1H), 3.05 (m, 2H), 2.87 (m, 2H), 2.65 (dd, J=7, 7 Hz, 2H).

1. extractionextracted with CHCl3 (2×75 mL)
2. washThe organic solution was washed with saturated bicarbonate
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure