反应详情

温度

100 °C

A vial was charged 3-bromo-6-chloro-2-methoxypyridine(0.50 g, 2.2 mmol), pyrrolidin-3-ol (0.39 g, 4.5 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.10 g, 0.10 mmol), Xantphos (0.13 g, 0.20 mmol), sodium tertbutoxide (0.32 g, 3.4 mmol) and toluene (5 mL). The mixture was purged with nitrogen then sealed. The mixture was heated to 100° C. overnight. The mixture was cooled to room temperature, filtered and diluted with 15 mL of water. The solution was extracted with ethyl acetate (10 mL×3). The organic layers were combined, dried over sodium sulfate, filtered and concentrated. The resulting residue was purified by silica gel chromatography to give the title compound (29.5 mg, 5.7%) as light brown solid.

1. customThe mixture was purged with nitrogen
2. customthen sealed
3. temperatureThe mixture was cooled to room temperature
4. filtrationfiltered
5. additiondiluted with 15 mL of water
6. extractionThe solution was extracted with ethyl acetate (10 mL×3)
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated
10. customThe resulting residue was purified by silica gel chromatography