反应 #45372
ord-c82eff29b5eb41a6a8ee7e33a5e62a24
反应条件
后处理
- 1过滤It was filtered
- 2浓缩the filtrate was concentrated
- 3workup.DISSOLUTIONThe residue was dissolved in methylene chloride
- 4洗涤washed with 1 N sodium hydroxide
- 5干燥dried over anhydrous sodium sulfate
- 6过滤filtered
- 7浓缩concentrated
实验过程
A mixture of silver sulfate (1.15 g, 3.68 mmol) and iodine (0.93 g, 3.68 mmol) were stirred in methanol at room temperature. A solution of p-ethylanisole (0.50 g, 3.68 mmol) in methanol was added dropwise to the stirring mixture. The mixture was stirred at room temperature until completion of the reaction. It was filtered and the filtrate was concentrated. The residue was dissolved in methylene chloride, washed with 1 N sodium hydroxide, dried over anhydrous sodium sulfate, filtered and concentrated. The title compound was obtained without further purification. 1H NMR (CDCl3, 500 MHz) δ 7.64 (d, J=2.0 Hz, 1H), 7.15 (dd, J=8.5, 2.0 Hz, 1H), 6.77 (d, J=8.0 Hz, 1H), 3.88 (s, 3H), 2.58 (q, J=15.5, 8.0 Hz, 2H), 1.23 (t, J=7.5 Hz, 3H).