反应详情

To a −78° C. solution of 2-(5-bromo-2-fluoro-phenyl)-[1,3]dioxolane (1.024 g, 4.047 mmol) in THF (40 mL) was added 2.5 M n-BuLi (1.80 mL, 4.45 mmol). After 20 min, the reaction was quenched with DMF (1.60 mL). After stirring for 1 h, the mixture was diluted with DCM, washed with a satd. aq. NaHCO3, dried (MgSO4), and concentrated. Purification by FCC (EtOAc/hexanes) gave the desired product (406.5 mg, 87%) as a white solid. 1H NMR (acetone-d6): 10.05 (s, 1H), 8.17-8.09 (m, 1H), 8.06-7.97 (m, 1H), 7.43-7.33 (m, 1H), 6.10-6.04 (m, 1H), 4.19-4.11 (m, 2H), 4.08-4.00 (m, 2H).

1. customthe reaction was quenched with DMF (1.60 mL)
2. additionthe mixture was diluted with DCM
3. washwashed with a satd
4. dry with materialaq. NaHCO3, dried (MgSO4)
5. concentrationconcentrated
6. customPurification by FCC (EtOAc/hexanes)