反应详情

To a solution of 20.0 g of 4-fluoro-3-nitro-benzoic acid methyl ester in 100 ml of abs. DMF was added 27.8 g of potassium carbonate, followed by 12.5 g of 2-methylcyclohexylamine. After 16 h at rt, the mixture was poured into water, the pH was adjusted to 4 by the addition of 2 M aqueous hydrochloric acid, and the reaction mixture was extracted with ethyl acetate three times. The combined organic phases were washed with water, dried over sodium sulphate and concentrated to yield 29.4 g (100%) of 4-(2-Methyl-cyclohexylamino)-3-nitro-benzoic acid methyl ester. C15H20N2O4 (292.34), LCMS (method 7—1—1): Rt=1.85 min, m/z=293.25 [M+H]+

1. extractionthe reaction mixture was extracted with ethyl acetate three times
2. washThe combined organic phases were washed with water
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated