反应详情

To a solution of 9a (0.7 g, 2.3 mmol) in CH2Cl2 (15 mL), TFA (2 mL) was added. The reaction mixture was stirred at room temperature for 4 h. The solvent was removed under reduced pressure and the residue was neutralized with aqueous NaOH solution and extracted with CH2Cl2 (2×15 mL). The organic layer was washed with brine, dried and concentrated to give the crude product. The crude product was purified with column chromatography to afforded 10a (0.33 g, 70%). 1H NMR (CDCl3): δ 1.62-1.87 (m, 6H), 2.63 (s, 3H), 2.77 (m, 2H), 3.16-3.22 (m, 2H), 3.33 (m, 1H), 7.27 (d, J=8.4 Hz, 1H), 8.12 (dd, J=8.1, 2.4 Hz, 1H), 9.04 (d, J=2.4 Hz, 1H).

1. customThe solvent was removed under reduced pressure
2. extractionextracted with CH2Cl2 (2×15 mL)
3. washThe organic layer was washed with brine
4. customdried
5. concentrationconcentrated
6. customto give the crude product
7. customThe crude product was purified with column chromatography