反应详情

温度

70 °C

To a 100 mL round bottom flask was added phthalazine-5-carboxylic acid (0.50 g, 2.9 mmol) 1,1′-carbonyldiimidazole (0.93 g, 5.7 mmol) and DMF (2.2 mL). The mixture was stirred at 70° C. for 1 hour and treated with thiosemicarbazide (0.81 g, 8.9 mmol). The resulting mixture was stirred at 70° C. for 30 minutes. The mixture was concentrated under vacuum to remove almost all of the DMF. The remaining residue was treated with 2 N HCl with stirring until the solution reached pH 4. Upon standing, a yellow solid formed. The precipitate was recovered by filtration, washing with water and air dried to provide 1-(phthalazine-5-carbonyl)thiosemicarbazide (0.45 g, 63%).

1. stirringThe resulting mixture was stirred at 70° C. for 30 minutes
2. concentrationThe mixture was concentrated under vacuum
3. customto remove almost all of the DMF
4. additionThe remaining residue was treated with 2 N HCl
5. stirringwith stirring until the solution
6. customa yellow solid formed
7. filtrationThe precipitate was recovered by filtration
8. washwashing with water and air
9. customdried