反応 #161539

ord-43e68112a7e5497784c2a5353ee7bb7c

試薬

なし

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction mixture was concentrated under reduced pressure
  2. 2
    その他then triturated with diethyl ether
  3. 3
    ろ過The suspension was filtered
  4. 4
    濃縮the filtrate was concentrated under reduced pressure
  5. 5
    その他Purification by flash chromatography (100% hexanes)

実験手順

Coupling of 3-bromophenol (17) (5.0 g, 28.9 mmol) with 2-ethylbutan-1-ol (3.25 g, 31.79 mmol) was conducted following the procedure given for Example 6. The reaction mixture was concentrated under reduced pressure then triturated with diethyl ether. The suspension was filtered and the filtrate was concentrated under reduced pressure. Purification by flash chromatography (100% hexanes) gave 1-bromo-3-(2-ethylbutoxy)benzene a clear liquid. Yield (5.04 g, 62%): 1H NMR (400 MHz, DMSO-d6) δ 7.20 (t, J=8.0 Hz, 1H), 7.11 (t, J=2.2 Hz, 1H), 7.07 (dd, J=8.0, 2.0 Hz, 1H), 6.92 (dd, J=8.4, 2.6 Hz, 1H), 3.84 (d, J=5.6 Hz, 2H), 1.61-1.53 (m, 1H), 1.46-1.30 (m, 4H), 0.86 (t, J=7.4 Hz, 6H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08829244B2uspto-grants-2014_09