反应详情

A mixture of 3-benzyloxy-6-bromopyridin-2-ylamine (1.0 g, 3.6 mmol) and chloroacetaldehyde (1.2 mL, 50 wt. % in water) in IMS (12 mL) was stirred at reflux for 1 hour, then concentrated under reduced pressure. The residue was partitioned between an aqueous saturated solution of sodium bicarbonate and EtOAc. The organic layer was separated and washed with brine, dried over Na2SO4, filtered and concentrated. The residue was purified by flash chromatography (Si—PPC, MeOH:Et2O, gradient 0:100 to 1:99) to give 8-Benzyloxy-5-bromo-imidazo[1,2-a]pyridine as an beige solid (960 mg, 88%). LCMS (Method H) RT 3.08 min; [M+H]+ 303 (79Br) and 305 (81Br)

1. temperatureat reflux for 1 hour
2. concentrationconcentrated under reduced pressure
3. customThe residue was partitioned between an aqueous saturated solution of sodium bicarbonate and EtOAc
4. customThe organic layer was separated
5. washwashed with brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was purified by flash chromatography (Si—PPC, MeOH:Et2O, gradient 0:100 to 1:99)