反应详情

To the product of Example 10i (130 mg, 0.47 mmol) in acetic acid (2 mL) was added platinum dioxide (20 mg) and the reaction mixture was stirred under an atmosphere of hydrogen for 3 hours. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was diluted with saturated aqueous sodium bicarbonate and the aqueous layer was extracted with ethyl acetate. The organic phase was washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to afford the title compound (59 mg, Yield: 42%). 1H NMR (400 MHz, CDCl3) δ 7.50 (s, 1H), 7.49 (d, J=8.0 Hz, 1H), 7.06 (d, J=8.0 Hz, 1H), 5.77 (s, 1H), 4.11 (s, 2H), 3.21 (t, J=5.6 Hz, 2H), 2.90 (t, J=5.6 Hz, 2H), 2.32 (s, 1H), 1.58 (s, 4H), 1.24 (s, 6H), 1.05 (s, 6H) ppm.

1. filtrationThe mixture was filtered
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionThe residue was diluted with saturated aqueous sodium bicarbonate
4. extractionthe aqueous layer was extracted with ethyl acetate
5. washThe organic phase was washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by silica gel column chromatography