反应详情

CDI (1.8 g, 114 mmol) was added to a solution of ethyl 2-((2-amino-5-bromopyridin-3-yl)methylamino)acetate (1.1 g, 38.17 mmol) in dioxane (36 mL). The reaction mixture was stirred at reflux for 5 hours and then concentrated to dryness. The residue was partitioned between dichloromethane (40 mL) and water (30 mL). The aqueous phase was separated and extracted with dichloromethane (2×30 mL). The combined organic phases were washed with brine (50 mL), dried over sodium sulfate, filtered and concentrated to dryness. The isolated compound was finally precipitated from a mixture dichloromethane/pentane to give the title product as a yellow solid (670 mg, 56%).

1. temperatureat reflux for 5 hours
2. concentrationconcentrated to dryness
3. customThe residue was partitioned between dichloromethane (40 mL) and water (30 mL)
4. customThe aqueous phase was separated
5. extractionextracted with dichloromethane (2×30 mL)
6. washThe combined organic phases were washed with brine (50 mL)
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated to dryness
10. customThe isolated compound was finally precipitated from a mixture dichloromethane/pentane