反应详情

温度

80 °C

To a solution of 290 mg of 6-fluoro-3-[(E)-2-(4-fluorophenyl)-vinyl]-5-nitro-1-trityl-1H-indazole in a mixture of 5 mL N,N-dimethylformamide/9 mL methanol/1 mL water were added 30 mg of ammonium chloride and 150 mg of iron powder, and stirred at 80° C. for 8 hours. After filtering off the insoluble substances through Celite, the solvent was evaporated, and the resultant residue was dissolved in 15 mL of ethyl acetate. The organic layer was washed successively with water, saturated aqueous sodium hydrogen carbonate and saturated brine. After drying over anhydrous magnesium sulfate, the solvent was evaporated, to afford 252 mg of the title compound as pale brown non-crystalline powder.

1. filtrationAfter filtering off the insoluble substances through Celite
2. customthe solvent was evaporated
3. dissolutionthe resultant residue was dissolved in 15 mL of ethyl acetate
4. washThe organic layer was washed successively with water, saturated aqueous sodium hydrogen carbonate and saturated brine
5. dry with materialAfter drying over anhydrous magnesium sulfate
6. customthe solvent was evaporated