반응 #624672

반응 방정식

2-chloro-5-nitropyrimidine

4-(trifluoromethyl)-1H-pyrazole

K2CO3

→

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

수율 49.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   여과Potassium carbonate filtered off with a büchner funnel
2. 2
   기타acetonitrile removed under reduced pressure
3. 3
   workup.DISSOLUTIONThe crude material was dissolved in ethyl acetate
4. 4
   기타transferred to a separatory funnel
5. 5
   세척Organics washed with water (3×), with brine (1×)
6. 6
   건조dried over sodium sulfate
7. 7
   여과filtered
8. 8
   농축concentrated
9. 9
   기타to afford the raw material
10. 10
    기타Purification by silica gel flash chromatography (ethyl acetate/heptane)

실험 절차

A round bottom flask was charged with 2-chloro-5-nitropyrimidine (2.50 g, 15.7 mmol), 4-(trifluoromethyl)-1H-pyrazole (2.35 g, 17.2 mmol), K2CO3 (4.33 g, 31.3 mmol) and acetonitrile (39 mL). The reaction was heated at 80° C. for 2 hours. Potassium carbonate filtered off with a büchner funnel and acetonitrile removed under reduced pressure. The crude material was dissolved in ethyl acetate and transferred to a separatory funnel. Organics washed with water (3×), with brine (1×), dried over sodium sulfate, filtered and concentrated to afford the raw material. Purification by silica gel flash chromatography (ethyl acetate/heptane) provide 5-nitro-2-(4-(trifluoromethyl)-1H-pyrazol-1-yl)pyrimidine (1.95 g, 49%) as a yellow solid. MS (M+1): 259.2.

출처