반응 #1563943

ord-a7adbb57ebae4983837159bbc90c1b01

용매

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture was quenched with 1M aq
  2. 2
    추출NaOH solution, extracted with diethyl ether (3×100 mL)
  3. 3
    건조dried over anhydrous sodium sulphate
  4. 4
    농축concentrated under reduced pressure
  5. 5
    기타to afford the crude, which
  6. 6
    기타was purified by column chromatography (using silica gel and 2% ethyl acetate in hexane as eluent)

실험 절차

1-bromo-2-methoxyethane (5.49 g, 39.5 mmol) was added to a mixture of 2-bromo-4-fluoro phenol (5 g, 26.18 mmol) and K2CO3 (11.5 g, 83.25 mmol) in CH3CN (41.5 mL) and continued stirring at 80° C. for 16 hr. The reaction mixture was quenched with 1M aq.NaOH solution, extracted with diethyl ether (3×100 mL), dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford the crude, which was purified by column chromatography (using silica gel and 2% ethyl acetate in hexane as eluent) to afford the desired compound (Int-42). 1H NMR (300 MHz, CDCl3) δ ppm 7.3 (1H, m), 6.9 (1H, m), 6.7 (1H, m), 4.1 (2H, t), 3.8 (2H, t), 3.5 (3H, s).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09402833B2uspto-grants-2016_08