Reaktion #601671

ord-470cf675cae64eb1bbf473bbe2a1cd1d

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe mixture was then purged with nitrogen
  2. 2
    FiltrationThe reaction mixture was filtered
  3. 3
    Extraktionthe filtrate was then extracted with ethyl acetate
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigepurified by flash column chromatograph

Vorschrift

Charged (2-bromo-4-fluorophenyl)methanol (954 mg, 4.65 mmol), 4-fluoro-1-vinylbenzene (1.14 g, 9.31 mmol), Pd(PPh3)2Cl2 (49 mg, 0.07 mmol), Et3N (942 mg, 9.31 mmol) and DMF (5 mL) to a sealed tube, the mixture was then purged with nitrogen, heated to 150° C. for 3 h in microwave oven. The reaction mixture was filtered, the filtrate was then extracted with ethyl acetate, concentrated and purified by flash column chromatograph to give 569 mg of the title compound (50%). 1H NMR (400 MHz, CDCl3): δ 1.60 (1H, t, J=6.4 Hz), 4.78 (2H, d, J=6.4 Hz), 6.93-7.08 (4H, m), 7.31-7.35 (3H, m), 7.48-7.52 (2H, m).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09107916B2uspto-grants-2015_08