反应详情

To a stirring solution of methyl 2-amino-3-nitro-4-(trifluoromethyl)benzoate (5.80 g, 0.022 mol), ammonium formate (30.0 g, 0.476 mol) in ethanol (300 ml) was added 10% palladium on carbon (500 mg) at room temperature and stirred for 2 h. Insoluble was filtered off and filtrates were concentrated in vacuo. The residue was diluted with water and extracted with ethyl acetate. The extracts were washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel with a 20% ethyl acetate/n-hexane to give 5.10 g (0.022 mol, 99%) of the title compound as a yellow powder.

1. filtrationInsoluble was filtered off
2. concentrationfiltrates were concentrated in vacuo
3. additionThe residue was diluted with water
4. extractionextracted with ethyl acetate
5. washThe extracts were washed with water
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by column chromatography on silica gel with a 20% ethyl acetate/n-hexane