反应详情

To an ice-cooled nitric acid (fuming) (20 ml) was added methyl 2-(acetylamino)-4-(trifluoromethyl)benzoate (7.30 g, 0.028 mol) portionwise and stirred for 30 min. The reaction mixture was poured into ice-water and extracted with ethyl acetate. The extracts were washed with aqueous saturated sodium bicarbonate and water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel with a 30% ethyl acetate/n-hexane to give 3.20 g (0.010 mol, 38%) of the title compound as a yellow powder.

1. extractionextracted with ethyl acetate
2. washThe extracts were washed with aqueous saturated sodium bicarbonate and water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by column chromatography on silica gel with a 30% ethyl acetate/n-hexane