反应详情

4-Acetyl-2-t-butyl-5-dimethylamino-3(2H)-pyridazinone (2.5 g) was added to hydrazine (3.2 g)/ethanol (30 ml) and the mixture was refluxed for 6 hours. After the ethanol-hydrazine was distilled off, the residue was 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 diethyl ether and dried. White powder, 1.7 g. 1H-NMR (CDCl3) 6: 1.70(9H,s), 2.74(3H,s), 8.10(1H,s).

1. temperaturethe mixture was refluxed for 6 hours
2. distillationAfter the ethanol-hydrazine was distilled off
3. extractionthe residue was extracted with ethyl acetate
4. washThe organic layer was washed with saturated aqueous NaCl solution
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated to dryness
7. washThe residue was washed with n-hexane and diethyl ether
8. customdried