反应 #45372

ord-c82eff29b5eb41a6a8ee7e33a5e62a24

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤It was filtered
  2. 2
    浓缩the filtrate was concentrated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in methylene chloride
  4. 4
    洗涤washed with 1 N sodium hydroxide
  5. 5
    干燥dried over anhydrous sodium sulfate
  6. 6
    过滤filtered
  7. 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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737295B2uspto-grants-2010_06