反应详情

温度

80 °C

To a solution of 600 mg of 3-bromo-6-fluoro-5-nitro-1-trityl-1H-indazole in 6 mL of N,N-dimethylformamide were successively added 292 mg of 4-fluorostyrene, 71 mg of 2-(di-tert-butylphosphino)biphenyl, 27 mg of palladium acetate (II) and 0.85 mL of triethylamine, and stirred at 80° C. for 6.5 hours. The solvent was evaporated, and the resulting residue was dissolved in 25 mL of ethyl acetate. The organic layer was successively washed with water (twice) and saturated brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated. The obtained crude crystal was recrystallized from ethyl acetate-diisopropylether, to afford 304 mg of the title compound as bright yellow crystals.

1. customThe solvent was evaporated
2. dissolutionthe resulting residue was dissolved in 25 mL of ethyl acetate
3. washThe organic layer was successively washed with water (twice) and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was evaporated
6. customThe obtained crude crystal
7. customwas recrystallized from ethyl acetate-diisopropylether