반응 #45372

ord-c82eff29b5eb41a6a8ee7e33a5e62a24

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과It was filtered
  2. 2
    농축the filtrate was concentrated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in methylene chloride
  4. 4
    세척washed with 1 N sodium hydroxide
  5. 5
    건조dried over anhydrous sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737295B2uspto-grants-2010_06