反应详情

Phosphorus oxychloride (6.5 g) was added dropwise to DMF (15 ml) with ice-cooling and the mixture was stirred at room temperature for 30 minutes. Then, 2-t-butyl-5-dimethylamino-3(2H)-pyridazinone (3.3 g)/DMF (40 ml) was added dropwise with ice-cooling and the mixture was stirred at 70° C. for 1 hour. This reaction mixture was poured gradually into ice-NaHCO3 /water and extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. The residue was washed with n-hexane and dried. Yellow powder, 3.7 g. 1H-NMR (CDCl3) δ: 1.63(9H,s), 3.10(6H,s), 7.71(1H,s), 10.27(1H,s).

1. temperaturecooling
2. temperaturecooling
3. stirringthe mixture was stirred at 70° C. for 1 hour
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with saturated aqueous NaCl solution
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated to dryness
8. washThe residue was washed with n-hexane
9. customdried