反应详情

温度

85 °C

To a stirred solution of methyl 4-amino-2-(trifluoromethyl)nicotinate (1.97 g, 8.97 mmol) in dioxane/methanol/water (3:2:1 ratio by volume) is added lithium hydroxide (0.365 g, 15.2 mmol). The mixture was heated at 85° C. for 8 hours. The reaction mixture was cooled to room temperature and conc. HCl was added dropwise to adjust the pH to 2-3. Saturated NaCl solution was added. The aqueous layer is extracted with ethyl acetate (12×). The organic layer is washed with water, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to afford 1.75 g (95%) of 4-amino-2-(trifluoromethyl)nicotinic acid as a yellow solid. 1H NMR (400 MHz, CD3OD), 8.09 (d, 1H), 6.93 (d, 1H), LC/MS (M+1)=207.1.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionThe aqueous layer is extracted with ethyl acetate (12×)
3. washThe organic layer is washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo