Reaktion #601671
ord-470cf675cae64eb1bbf473bbe2a1cd1d
Reaktionsgleichung
Lösungsmittel
Reaktionsbedingungen
Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigethe mixture was then purged with nitrogen
- 2FiltrationThe reaction mixture was filtered
- 3Extraktionthe filtrate was then extracted with ethyl acetate
- 4Einengenconcentrated
- 5Sonstigepurified 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).