反応 #44787

ord-c4f73b96e4cc4bb3806897b156366a96

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度The reaction was heated
  3. 3
    温度at reflux for 2 days
  4. 4
    濃縮The reaction was concentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
  6. 6
    洗浄washed with water
  7. 7
    その他The combined organic layers were dried
  8. 8
    濃縮concentrated
  9. 9
    その他The residue was recrystallized from methanol

実験手順

A solution of 2-[4-[[4-(2-chloroethoxy)phenyl]methyl]phenyl]oxazole (1.7 g, 4.4 mmol) in 2-butanone (18 mL) was stirred as sodium iodide (7 g, 44 mmol) was added. The reaction was heated at reflux for 2 days. The reaction was concentrated. The residue was dissolved in ethyl acetate and washed with water. The combined organic layers were dried and concentrated. The residue was recrystallized from methanol to give 1.4 g of 2-[4-[[4-(2-iodoethoxy)phenyl]methyl]phenyl]oxazole, 1H NMR (400 MHz, CDCl3) δ 7.97 (d, 2H), 7.68 (s, 1H), 7.27 (d, 2H), 7.21 (s, 1H), 7.13 (d, 2H), 6.82 (d, 2H), 4.22 (t, 2H), 3.96 (s, 2H), 3.39 (t, 2H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07737145B2uspto-grants-2010_06