反応 #59492

ord-7f9a6aad03f3423b9c5a65a32fd0e897

反応条件

温度
22°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The mixture was filtered
  2. 2
    その他evaporated to dryness under reduced pressure
  3. 3
    その他The residue was triturated with the mixture of ether (8.2 ml) and water (1.4 ml) at the ice bath temperature
  4. 4
    ろ過The product was collected by filtration
  5. 5
    洗浄washed with cold ether
  6. 6
    その他dried under reduced pressure

実験手順

A mixture of 2,5-bis(benzyloxy)phenol (0.28 g), 2-bromoacetophenone (0.22 g), potassium hydrogen-carbonate (0.25 g) and 18-Crown-6 (3 mg) in acetonitrile (4.2 ml) was stirred at 22° C. for one week. The mixture was filtered and evaporated to dryness under reduced pressure. The residue was triturated with the mixture of ether (8.2 ml) and water (1.4 ml) at the ice bath temperature. The product was collected by filtration, washed with cold ether and dried under reduced pressure. Yield is 0.14 g. 1H NMR (DMSO-d6) δ=4.98 (s, 2H), 5.06 (s, 2H), 5.58 (s, 2H), 6.51 (dd, J=8.9, 2.3 Hz, 1H), 6.68 (d, J=2.3 Hz, 1H), 6.94 (d, J=8.9 Hz, 1H), 7.28-8.03 (m, 15H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07425568B2uspto-grants-2008_09