Reaktion #62409

Reaktionsgleichung

5-bromo-6-fluoro-3-iodo-1-trityl-1H-indazole

4-fluorostyrene

2-(di-ter-butylphosphino)biphenyl

triethylamine

→

title compound

Ausbeute 74.1%

5-Bromo-6-fluoro-3-[(E)-2-(4-fluorophenyl)vinyl]-1-trityl-1H-indazole

Ausbeute 74.1%

Lösungsmittel

ethyl acetate

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashing successively with aqueous ammonium chloride and saturated brine
2. 2
   Trocknendrying over anhydrous magnesium sulfate
3. 3
   Sonstigethe solvent was evaporated
4. 4
   SonstigeThe residue was purified
5. 5
   Sonstigeseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:100)

Vorschrift

A solution of 3.0 g of 5-bromo-6-fluoro-3-iodo-1-trityl-1H-indazole, 628 mg of 4-fluorostyrene, 115 mg of palladium acetate, 307 mg of 2-(di-ter-butylphosphino)biphenyl and 3.60 mL of triethylamine in N,N-dimethylformamide was stirred at 70° C. for a day. After diluting with ethyl acetate, washing successively with aqueous ammonium chloride and saturated brine, and drying over anhydrous magnesium sulfate, the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:100), to afford 2.2 g of the title compound as colorless crystals.

Quelle