反应详情

温度

80 °C

To a solution of 2-chloro-5-nitropyrimidine (1.5 g, 9.4 mmol) and 4-(trifluoromethyl)-1H-pyrazole (1.41 g, 10.3 mmol) in acetonitrile (40 mL) was added potassium carbonate (2.60 g, 18.8 mmol). The reaction was heated to 80° C. and stirred overnight. The reaction was concentrated and the residue was diluted with water and extracted with ethyl acetate (2×40 mL). The combined organics were washed with brine, dried over sodium sulfate, filtered, and concentrated. Purification by flash column chromatography gave 5-nitro-2-(4-(trifluoromethyl)-1H-pyrazol-1-yl)pyrimidine (1.5 g, 62%) as a yellow solid. 1H NMR (400 MHz, CDCl3, δ): 9.48 (s, 2H), 8.92 (s, 1H), 8.05 (s, 1H).

1. concentrationThe reaction was concentrated
2. additionthe residue was diluted with water
3. extractionextracted with ethyl acetate (2×40 mL)
4. washThe combined organics were washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by flash column chromatography