反应详情

温度

90 °C

A mixture of the chloride (Intermediate II, 420 mg, 1.69 mmol) and potassium carbonate (818 mg, 5.92 mmol) in 2-methoxyethanol (12 ml) was stirred for 2 hours at 90° C. TLC indicated complete conversion. The mixture was filtered through a pad of celite and the solvent was removed under vacuum. The residue was purified by column chromatography (silica gel, ethyl acetate/heptane, 25-70% gradient) to give 46% (225 mg, 781 μmol) of title compound as pale yellow oil. 1H NMR (300 MHz, CDCl3) δ 1.56 (s, 9H), 3.39 (s, 3H), 3.54-3.58 (m, 2H), 3.64-3.69 (m, 2H), 4.58 (s, 2H), 6.82 (s, 1H).

1. filtrationThe mixture was filtered through a pad of celite
2. customthe solvent was removed under vacuum
3. customThe residue was purified by column chromatography (silica gel, ethyl acetate/heptane, 25-70% gradient)