反应详情

To a stirred solution of 2-methyl-4-(1H-pyrazol-1-yl)pyridine (300 mg, 1.9 mmol) in CCl4 (25 mL), N-bromo succinimide (304 mg, 1.71 mmol) and benzoyl peroxide (23 mg, 0.09 mmol) were added and heated to reflux for 16 h. The reaction mixture was cooled to rt and precipitated succinimide was filtered. The filtrate was absorbed on silicagel and concentrated under reduced pressure. The crude product was purified flash column chromatography (eluent: 5% ethyl acetate in hexane) to yield the title compound (100 mg, 45%). [TLC Rf=0.34 (ethyl acetate/hexane 30:70)].

1. temperatureheated
2. temperatureto reflux for 16 h
3. customprecipitated succinimide
4. filtrationwas filtered
5. customThe filtrate was absorbed on silicagel and
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified flash column chromatography (eluent: 5% ethyl acetate in hexane)