反应详情

To a solution of (3-bromo-5-fluorophenyl)methanol (4 g, 19.51 mmol) in DCM (39.0 mL) at 0° C., DAST (3.35 mL, 25.4 mmol) was added. The reaction mixture was allowed to return to room temperature and stirred at room temperature overnight. Sat. NaHCO3 was added, the reaction mixture was then extracted by DCM. The organic was dried and concentrated. The crude material was purified by flash chromatography (0-10% EtOAc/heptanes) to yield the final product as colorless oil. LCMS (m/z): no mass (MH+), 0.86 min. 1H NMR (400 MHz, CDCl3) δ ppm 7.30 (s, 1H), 7.23 (d, J=8.2 Hz, 1H), 7.03 (d, J=8.6 Hz, 1H), 5.41 (s, 1H), 5.29 (s, 1H).

1. customto return to room temperature
2. extractionthe reaction mixture was then extracted by DCM
3. customThe organic was dried
4. concentrationconcentrated
5. customThe crude material was purified by flash chromatography (0-10% EtOAc/heptanes)