반응 #62409

반응 방정식

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

4-fluorostyrene

2-(di-ter-butylphosphino)biphenyl

triethylamine

→

title compound

수율 74.1%

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

수율 74.1%

용매

ethyl acetate

N,N-dimethylformamide

반응 조건

후처리

1. 1
   세척washing successively with aqueous ammonium chloride and saturated brine
2. 2
   건조drying over anhydrous magnesium sulfate
3. 3
   기타the solvent was evaporated
4. 4
   기타The residue was purified
5. 5
   기타separated by silica gel column chromatography (ethyl acetate:n-hexane=1:100)

실험 절차

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.

출처