反应详情

A mixture of 2-chloro-5-iodopyridine (1.918 g, 8.01 mmol), anhydrous hydrazine (1.26 mL, 40.05 mmol) and pyridine (30 mL) was warmed at reflux for 18 h. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. The residue was partitioned between dichloromethane and 1N aqueous sodium hydroxide solution. The organic layer was separated, dried (magnesium sulfate) and concentrated under reduced pressure. The residue was triturated with hexanes, and the resultant precipitate was collected and dried in vacuo to afford the title compound as off-white crystals. LC/MS 235.8 (M+1).

1. temperaturewas warmed
2. temperatureat reflux for 18 h
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. customThe residue was partitioned between dichloromethane and 1N aqueous sodium hydroxide solution
5. customThe organic layer was separated
6. dry with materialdried (magnesium sulfate)
7. concentrationconcentrated under reduced pressure
8. customThe residue was triturated with hexanes
9. customthe resultant precipitate was collected
10. customdried in vacuo