반응 #624660

반응 방정식

5-bromo-2-chloro-3-methylpyridine

4-(trifluoromethyl)-1H-pyrazole

potassium carbonate

→

5-bromo-3-methyl-2-(4-(trifluoromethyl)-1H-pyrazol-1-yl)pyridine

수율 30.0%

용매

dimethylformamide

반응 조건

후처리

1. 1
   농축The reaction was concentrated
2. 2
   기타to give 690 mg of crude material
3. 3
   기타Purification by silica gel flash chromatography (0-5% ethyl acetate in heptane)

실험 절차

A flask was charged with 5-bromo-2-chloro-3-methylpyridine (250 mg, 1.21 mmol), 4-(trifluoromethyl)-1H-pyrazole (165 mg, 1.21 mmol), potassium carbonate (512 mg, 3.63 mmol), and anhydrous dimethylformamide (1.21 mL). The reaction was heated at 85 to 130° C. for 36 h. The reaction was concentrated to give 690 mg of crude material. Purification by silica gel flash chromatography (0-5% ethyl acetate in heptane) afforded 5-bromo-3-methyl-2-(4-(trifluoromethyl)-1H-pyrazol-1-yl)pyridine (containing approximately 30% starting material) was carried forth to the next reaction. MS (M+1) 308.1.

출처