반응 #45372
ord-c82eff29b5eb41a6a8ee7e33a5e62a24
반응 조건
후처리
- 1여과It was filtered
- 2농축the filtrate was concentrated
- 3workup.DISSOLUTIONThe residue was dissolved in methylene chloride
- 4세척washed with 1 N sodium hydroxide
- 5건조dried over anhydrous sodium sulfate
- 6여과filtered
- 7농축concentrated
실험 절차
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).