反应详情

To a suspension of (E)-methyl 6-(2-((8-tert-butylquinolin-2-yl)methylene)hydrazinyl)nicotinate (1.78 g, 4.91 mmol) in DCM (40 mL) was added iodobenzene diacetate (1.90 g, 5.89 mmol). The reaction mixture was stirred at ambient temperature for 4 hours. The solvent was removed, and the resulting residue was suspended in 1:1 hexane/ether (50 mL) and stirred at ambient temperature for 10 minutes. The solid that formed was collected by filtration. The solid was then suspended in 1:1 THF/H2O (50 mL) and LiOH—H2O (0.82 g, 19.6 mmol) was added. The reaction mixture was stirred at ambient temperature for 2 hours. THF was removed under reduced pressure. The resulting aqueous solution was acidified with saturated potassium hydrogen sulfate to pH˜3-4. The solid that formed was collected by filtration, washed with water, 1:1 hexane/ether (50 mL) and dried to give 3-(8-tert-butylquinolin-2-yl)-[1,2,4]triazolo[4,3-a]pyridine-6-carboxylic acid (1.55 g, 91.1%) as solid.

1. customThe solvent was removed
2. stirringstirred at ambient temperature for 10 minutes
3. customThe solid that formed
4. filtrationwas collected by filtration
5. additionwas added
6. stirringThe reaction mixture was stirred at ambient temperature for 2 hours
7. customTHF was removed under reduced pressure
8. customThe solid that formed
9. filtrationwas collected by filtration
10. washwashed with water, 1:1 hexane/ether (50 mL)
11. customdried