反应详情

A mixture of 2-bromo-4-methoxyphenol (1.50 g, 7.39 mmol) (Bionet, CAS# 17332-11-5), 1-bromobutane (0.95 mL, 8.87 mmol) (Acros, CAS# 109-65-9), and cesium carbonate (3.13 g, 9.60 mmol) in DMF (40 mL) was stirred overnight at room temperature. The mixture was diluted with EtOAc, washed with water and brine, dried over Na2SO4, and concentrated. The crude product was purified by silica gel flash chromatography (0-20% EtOAc/hexane) to afford compound C.2 (1.49 g, 78% yield) as a colorless oil. 1H NMR (400 MHz, CDCl3) δ 7.15 (d, J=2.7 Hz, 1H), 6.84 (d, J=9.0 Hz, 1H), 6.80 (dd, J=3.1, 9.0 Hz, 1H), 3.97 (t, J=6.5 Hz, 2H), 3.76 (s, 3H), 1.79 (m, 2H), 1.53 (m, 2H), 0.98 (t, J=7.2 Hz, 3H).

1. washwashed with water and brine
2. dry with materialdried over Na2SO4
3. concentrationconcentrated
4. customThe crude product was purified by silica gel flash chromatography (0-20% EtOAc/hexane)
5. customto afford compound C.2 (1.49 g, 78% yield) as a colorless oil