تفاعل #45372

ord-c82eff29b5eb41a6a8ee7e33a5e62a24

المتفاعلات

الكواشف

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحIt was filtered
  2. 2
    تركيزthe filtrate was concentrated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in methylene chloride
  4. 4
    غسيلwashed with 1 N sodium hydroxide
  5. 5
    تجفيفdried over anhydrous sodium sulfate
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737295B2uspto-grants-2010_06