반응 #624640

반응 방정식

2-chloro-5-nitropyrimidine

4-(trifluoromethyl)-1H-pyrazole

potassium carbonate

→

5-nitro-2-(4-(trifluoromethyl)-1H-pyrazol-1-yl)pyrimidine

수율 62.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   농축The reaction was concentrated
2. 2
   workup.ADDITIONthe residue was diluted with water
3. 3
   추출extracted with ethyl acetate (2×40 mL)
4. 4
   세척The combined organics were washed with brine
5. 5
   건조dried over sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated
8. 8
   기타Purification by flash column chromatography

실험 절차

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).

출처