反应详情

To a solution of 5.01 g of N-(5-fluoro-2-methyl-phenyl)-acetamide in 30 mL of concentrated sulfuric acid was added dropwise 2.74 g of 70% nitric acid (d=1.42) while keeping the inner temperature at 3° C. After stirring for 40 minutes at this temperature, the reaction solution was poured dropwise into ice water under stirring. After collecting the precipitated powder by filtration, the powder was dissolved in 100 mL of ethyl acetate, washed successively with saturated aqueous sodium hydrogen carbonate (twice) and saturated brine. After drying over anhydrous magnesium sulfate, the solvent was evaporated. The residue was crystallized from ethanol, to afford 3.68 g of the title compound as yellow needle crystals.

1. customat 3° C
2. stirringunder stirring
3. customAfter collecting the precipitated powder
4. filtrationby filtration
5. dissolutionthe powder was dissolved in 100 mL of ethyl acetate
6. washwashed successively with saturated aqueous sodium hydrogen carbonate (twice) and saturated brine
7. dry with materialAfter drying over anhydrous magnesium sulfate
8. customthe solvent was evaporated
9. customThe residue was crystallized from ethanol