反应详情

温度

150 °C

A vial was charged with 3-bromo-6-chloro-2-methoxypyridine (1.00 g, 4.5 mmol), rac-pyrrolidin-3-ol (0.59 g, 6.7 mmol), triethylamine (0.91 g, 8.9 mmol) and dimethylsulfoxide (4 mL). The mixture was heated to 150° C. for 5 hrs. The mixture was cooled to room temperature and diluted with 20 mL of water. The solution was extracted with ethyl acetate (10 mL×3). The extracts were combined, dried (sodium sulfate) and concentrated. The resulting residue was purified through flash column chromatography (petroleum ether/ethyl acetate=5:1˜2:1) to give the title compound (0.26 g, 25.3%) as light brown gum.

1. temperatureThe mixture was cooled to room temperature
2. extractionThe solution was extracted with ethyl acetate (10 mL×3)
3. dry with materialdried (sodium sulfate)
4. concentrationconcentrated
5. customThe resulting residue was purified through flash column chromatography (petroleum ether/ethyl acetate=5:1˜2:1)